Page 120 - 《精细化工》2022年第9期
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·1838· 精细化工 FINE CHEMICALS 第 39 卷
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熔点 57.5~58.3 ℃。HNMR(DMSO-d 6 ),δ:0.90〔m, 〔(CH 2) 7CH 2CH 2〕, 27.97〔(CH 2) 7〕, 29.37〔(CH 2) 7〕,
9H, CH 3 CH 2 , CH 3 CH 2 , (CH 2 ) 5 CH 3 〕, 1.05 (m, 2H, 31.76 (CH 2CH 2CH 2), 32.71 (CH 2CH 2), 35.55 (NHCH 2 ),
+
+
+
+
CH 2 CH 3 ), 1.24〔m, 8H, CH 2 (CH 2 ) 4 〕, 1.57〔m, 4H, 50.40 (CH 2 N ), 52.25 (N CH 2 , N CH 2 , N CH 2 ), 63.74
(CH 2 OH), 70.65 (CHOH), 71.92 (CHOH), 72.63
+
CH 2 CH 2 (CH 2 ) 5, N CH 2CH 2 〕, 1.77 (t, 2H, CH 2 CH 2CH 2 ), (CHOH), 73.98 (CHOH), 173.55 (CONH)。
2.92 (m, 4H, CH 3 CH 2 , CH 3 CH 2 ), 3.15 (m, 4H,
+
CH 2 CH 2 CH 2 , CH 2 CH 2 CH 2 ), 3.38 (t, 2H, CH 2 CH 2 N ), C 14 DGMAPB:收率:87.97%(淡黄色固体)。熔
1
+
+
3.50 (m, 4H, CH 2 CH 2 N , CH 2 CH 2 N ), 3.56 (m, 2H, 点 67.5~69.3 ℃。HNMR(DMSO-d 6),δ:0.91〔m, 9H,
NHCH 2 ), 3.78 (m, 1H, CHOH), 3.92 (m, 1H, CHOH), CH 3 CH 2 , CH 3CH 2 , (CH 2 ) 11 CH 3 〕, 1.06 (m, 2H, CH 2 CH 3 ),
4.01 (m, 1H, CHOH), 4.06 (m, 1H, CHOH), 4.16 (m, 1.25〔m, 22H, CH 2 (CH 2 ) 11 〕, 1.59〔m, 4H, CH 2 CH 2 (CH 2 ) 11 ,
2H, CH 2 OH), 4.42~5.46 (m, 5H, OH 为糖基上的羟 N CH 2CH 2 〕, 1.82 (t, 2H, CH 2 CH 2 CH 2 ), 2.96 (m, 4H,
+
13
基), 7.88 (t, 1H, CONH)。 CNMR(DMSO-d 6 ),δ: CH 3 CH 2 , CH 3 CH 2 ), 3.15 (m, 4H, CH 2 CH 2 CH 2 ,
13.93 (CH 3 , CH 3 , CH 3 ), 14.37 (CH 2 CH 3 ), 19.93 CH 2 CH 2 CH 2 ), 3.38 (t, 2H, CH 2 CH 2 N ), 3.51 (m, 4H,
+
(CH 3 CH 2 CH 2 , CH 3 CH 2 CH 2 ), 22.57 (CH 2 CH 2 , CH 2 CH 2 N , CH 2 CH 2 N ), 3.60 (m, 2H, NHCH 2 ), 3.72
+
+
CH 2 CH 2 ), 25.59〔(CH 2 ) 3 CH 2 CH 2 〕, 27.97 〔(CH 2 ) 3 〕, (m, 1H, CHOH), 3.93 (m, 1H, CHOH), 4.03 (m, 1H,
29.37〔(CH 2 ) 3 〕, 31.76 (CH 2 CH 2 CH 2 ), 32.71 (CH 2 CH 2 ), CHOH), 4.17 (m, 1H, CHOH), 4.42 (m, 2H, CH 2 OH),
+
+
35.55 (NHCH 2 ), 50.40 (CH 2 N ), 52.25 (N CH 2 , 4.55~5.50 (m, 5H, OH 为糖基上的羟基), 7.90 (t, 1H,
+
+
N CH 2 , N CH 2 ), 63.74 (CH 2 OH), 70.65 (CHOH), CONH)。 CNMR(DMSO-d 6),δ:13.99 (CH 3, CH 3, CH 3),
13
71.92 (CHOH), 72.63 (CHOH), 73.98 (CHOH), 14.37 (CH 2CH 3), 19.93 (CH 3CH 2CH 2, CH 3CH 2CH 2),
173.55 (CONH)。
22.57 (CH 2CH 2, CH 2CH 2), 25.59〔(CH 2 ) 9 CH 2 CH 2 〕,
C 10 DGMAPB:收率:89.47%(淡黄色固体)。 27.97〔(CH 2 ) 9 〕, 29.37〔(CH 2 ) 9 〕, 31.76 (CH 2 CH 2 CH 2 ),
1
HNMR(DMSO-d 6 ) , δ : 0.85 〔 m, 9H, CH 3 CH 2 , 32.71 (CH 2 CH 2 ), 35.55 (NHCH 2 ), 50.40 (CH 2 N ),
+
+
+
+
CH 3 CH 2 , (CH 2 ) 7 CH 3 〕, 1.09 (m, 2H, CH 2 CH 3 ), 1.24 52.25 (N CH 2 , N CH 2 , N CH 2 ), 63.74 (CH 2 OH),
〔m, 12H, CH 2 (CH 2 ) 6 〕, 1.58〔m, 4H, CH 2 CH 2 (CH 2 ) 7 , 70.65 (CHOH), 71.92(CHOH), 72.63 (CHOH), 73.98
+
N CH 2 CH 2 〕, 1.78 (t, 2H, CH 2 CH 2 CH 2 ), 2.96 (m, 4H, (CHOH), 173.55 (CONH)。
CH 3 CH 2 , CH 3 CH 2 ), 3.14 (m, 4H, CH 2 CH 2 CH 2 , C 16 DGMAPB:收率:86.87%(淡黄色固体)。
+
CH 2 CH 2 CH 2 ), 3.37 (t, 2H, CH 2 CH 2 N ), 3.49 (m, 4H, 熔点 69.3~70.9 ℃。HNMR(DMSO-d 6 ),δ:0.86〔m,
1
+
+
CH 2 CH 2 N , CH 2 CH 2 N ), 3.56 (m, 2H, NHCH 2 ), 3.74 9H, CH 3 CH 2 , CH 3 CH 2 , (CH 2 ) 11 CH 3 〕, 1.06 (m, 2H,
(m, 1H, CHOH), 3.91 (m, 1H, CHOH), 4.01 (m, 1H,
CHOH), 4.14 (m, 1H, CHOH), 4.41 (m, 2H, CH 2 OH), CH 2 CH 3 ), 1.25〔m, 24H, CH 2 (CH 2 ) 12 〕, 1.58〔m, 4H,
+
4.53~5.42 (m, 5H, OH 为糖基上的羟基), 7.88 (t, 1H, CH 2 CH 2 (CH 2 ) 13 , N CH 2 CH 2〕, 1.82 (t, 2H, CH 2 CH 2CH 2 ),
13
CONH)。 CNMR(DMSO-d 6),δ:13.99 (CH 3, CH 3, CH 3), 2.96 (m, 4H, CH 3 CH 2 , CH 3 CH 2 ), 3.16 (m, 4H,
+
14.37 (CH 2CH 3), 19.93 (CH 3CH 2CH 2, CH 3 CH 2 CH 2 ), CH 2 CH 2 CH 2 , CH 2 CH 2 CH 2 ), 3.38 (t, 2H, CH 2 CH 2 N ),
+
+
3.51 (m, 4H, CH 2 CH 2 N , CH 2 CH 2 N ), 3.58 (m, 2H,
22.57 (CH 2 CH 2 , CH 2 CH 2 ), 25.59〔(CH 2 ) 5 CH 2 CH 2 〕, NHCH 2 ), 3.77 (m, 1H, CHOH), 3.93 (m, 1H, CHOH),
27.97〔(CH 2 ) 5 〕, 29.37〔(CH 2 ) 5 〕, 31.76 (CH 2 CH 2 CH 2 ), 4.03 (m, 1H, CHOH), 4.18 (m, 1H, CHOH), 4.42 (m, 2H,
+
32.71 (CH 2 CH 2 ), 35.55 (NHCH 2 ), 50.40 (CH 2 N ), CH 2OH), 4.50~5.51 (m, 5H, OH 为糖基上的羟基), 7.90
+
+
+
52.25 (N CH 2 , N CH 2 , N CH 2 ), 63.74 (CH 2 OH), (t, 1H, CONH)。 CNMR (DMSO-d 6 ),δ:14.19 (CH 3 ,
13
70.65 (CHOH), 71.92 (CHOH), 72.63 (CHOH), 73.98 CH 3 , CH 3 ), 14.37 (CH 2 CH 3 ), 19.93 (CH 3CH 2CH 2,
(CHOH), 173.55 (CONH)。
CH 3CH 2CH 2), 22.57 (CH 2 CH 2 , CH 2 CH 2 ), 25.59
C 12 DGMAPB:收率:89.67%(淡黄色固体)。 〔(CH 2 ) 11 CH 2 CH 2 〕, 27.97〔(CH 2 ) 11 〕, 29.37〔(CH 2) 11〕,
1
熔点 66.6~67.3 ℃。HNMR(DMSO-d 6 ),δ:0.85〔m, 31.76 (CH 2CH 2CH 2), 32.71 (CH 2 CH 2 ), 35.55 (NHCH 2 ),
+
+
+
+
9H, CH 3CH 2, CH 3CH 2, (CH 2) 9CH 3 〕, 1.08 (m, 2H, 50.40 (CH 2 N ), 52.25 (N CH 2 , N CH 2 , N CH 2 ), 63.74
CH 2CH 3), 1.24〔m, 16H, CH 2(CH 2) 8〕, 1.57〔m, 4H, (CH 2 OH), 70.65 (CHOH), 71.92 (CHOH), 72.63
+
CH 2 CH 2 (CH 2 ) 9, N CH 2CH 2 〕, 1.75 (t, 2H, CH 2 CH 2CH 2 ), (CHOH), 73.98 (CHOH), 173.55 (CONH)。
2.92 (m, 4H, CH 3 CH 2 , CH 3 CH 2 ), 3.17 (m, 4H, 综合以上分析结果可知,已经成功制备出
+
CH 2 CH 2 CH 2 , CH 2 CH 2 CH 2 ), 3.38 (t, 2H, CH 2 CH 2 N ), DGMAPA 和 C n DGMAPB。
+
+
3.48 (m, 4H, CH 2 CH 2 N , CH 2 CH 2 N ), 3.56 (m, 2H, 2.2 表面张力分析
NHCH 2 ), 3.78 (m, 1H, CHOH), 3.92 (m, 1H, CHOH), C n DGMAPB 水溶液的表面张力如图 4 所示。由
4.01 (m, 1H, CHOH), 4.18 (m, 1H, CHOH), 4.39 (m,
2H, CH 2 OH), 4.54~5.51 (m, 5H, OH 为糖基上的羟 图 4 可知,当浓度小于 0.3 mmol/L 时表面活性剂溶
13
基), 7.86 (t, 1H, CONH)。 CNMR(DMSO-d 6),δ:13.20 液的表面张力随浓度的增加而急剧下降,并呈线性
(CH 3 , CH 3 , CH 3 ), 14.37 (CH 2 CH 3 ), 19.93 (CH 3 CH 2 CH 2 , 关系,当浓度达到一定值时出现转折点,此点所对
CH 3 CH 2 CH 2 ), 22.57 (CH 2 CH 2 , CH 2 CH 2 ), 25.59 应的浓度为临界胶束浓度(cmc),也意味着胶束