Page 236 - 《精细化工》2023年第4期

g922g ㇫㏳ࡃጒ FINE CHEMICALS す 40 ࢤ

3-㓌ധ-3-(2-⩟⅔ധ㠜ധ)͆䚥Ά䚜喍4喎喟叱㞟⇦ 113.79 (Ar-C), 64.09 (COH), 61.07 (CH 2 O), 41.77
+
1
⟣➖ [29] 喑188.8 mg喑ϔ⢴ 90%ȡ HNMR (400 MHz, (CH 2 ), 14.03 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ
CDCl 3 ), į: 7.34~7.31 (m, 1H, Ar-H), 7.17~7.10 (m, 230.09喠჋≸թ 230.08ȡ
1H, Ar-H), 6.87~6.83 (m, 1H, Ar-H), 6.75~6.73 (m, 3-㓌ധ-3-(2-⏡㠜ധ)͆䚥Ά䚜喍9喎喟叱㞟⇦⟣➖ [30] 喑
1H, Ar-H), 5.30~5.21 (m, 1H, CHOH), 4.04 (q, J = 7.2 234.0 mg喑ϔ⢴ 86%ȡ HNMR (400 MHz, CDCl 3 ), į:
1
Hz, 2H, OCH 2 ), 3.70 (s, 3H, OCH 3 ), 3.58 (s, 1H, OH),
2.74~2.52 (m, 2H, CH 2 ), 1.13 (t, J = 7.2 Hz, 3H, 7.26~7.23 (m, 2H, Ar-H), 6.96~6.91 (m, 2H, Ar-H),
5.01~4.99 (m, 1H, CHOH), 4.07 (q, J = 7.1 Hz, 2H,
13
CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į: 172.61 (O==C), OCH 2 ), 3.54 (s, 1H, OH), 2.67~2.53 (m, 2H, CH 2 ),
155.95 (Ar-C), 130.71 (Ar-C), 128.52 (Ar-C), 126.53 1.16 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR (101 MHz,
13
(Ar-C), 120.73 (Ar-C), 110.25 (Ar-C), 66.34 (COH), CDCl 3 ), į: 172.27 (O==C), 163.47 (Ar-C), 161.03
60.66 (CH 2 O), 55.21 (OCH 3 ), 41.83 (CH 2 ), 14.16 (Ar-C), 138.44 (Ar-C), 127.45 (Ar-C), 115.43 (Ar-C),
+
(CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 225.06喠჋≸
115.22 (Ar-C), 69.67 (COH), 60.95 (CH 2 O), 43.42
թ 225.06ȡ (CH 2 ), 14.10 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ
+
3-㓌ധ-3-(2-⅜㠜ധ)͆䚥Ά䚜喍5喎喟叱㞟⇦⟣➖ [26] 喑 274.03喠჋≸թ 274.01ȡ
1
209.8 mg喑ϔ⢴ 92%ȡ HNMR (400 MHz, CDCl 3 ), į: 3-㓌ധ-3-(2-㥅ധ)͆䚥Ά䚜喍10喎喟叱㞟⇦⟣➖ [26] 喑
7.25~7.19 (m, 4H, Ar-H), 5.02~4.99 (m, 1H, CHOH), 217.3 mg喑ϔ⢴ 89%ȡ HNMR (400 MHz, CDCl 3 ), į:
1
4.09 (q, J = 7.2 Hz, 2H, OCH 2 ), 3.50 (s, 1H, OH),
2.67~2.54 (m, 2H, CH 2 ), 1.17 (t, J = 7.2 Hz, 3H, 8.01 (d, J = 6.2 Hz, 1H, Ar-H), 7.86~7.78 (m, 1H,
13
CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į: 172.24 (O==C), Ar-H), 7.73~7.71 (m, 1H, Ar-H), 7.65 (d, J = 6.2 Hz,
1H, Ar-H), 7.49~7.37 (m, 3H, Ar-H), 5.88~5.85 (m,
141.09 (Ar-C), 133.43 (Ar-C), 128.67 (Ar-C), 127.11 1H, CHOH), 4.15 (q, J = 7.2 Hz, 2H, OCH 2 ), 3.66 (br,
(Ar-C), 69.63 (COH), 61.02 (CH 2 O), 43.26 (CH 2 ), 1H, OH), 2.87~2.72 (m, 2H, CH 2 ), 1.21 (t, J = 7.2 Hz,
+
14.14 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 228.10喑 13
3H, CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į: 172.71
჋≸թ 228.11ȡ (O==C), 138.26 (Ar-C), 133.77 (Ar-C), 130.01 (Ar-C),
3-㓌ധ-3-(4-⅜㠜ധ)͆䚥Ά䚜喍6喎喟叱㞟⇦⟣➖ [28] 喑 129.02 (Ar-C), 128.26 (Ar-C), 126.29 (Ar-C), 125.63
1
214.2 mg喑ϔ⢴ 94%ȡ HNMR (400 MHz, CDCl 3 ), į: (Ar-C), 125.55 (Ar-C), 123.01 (Ar-C), 122.88 (Ar-C),
7.24~7.19 (m, 4H, Ar-H), 5.01~4.99 (m, 1H, CHOH), 67.34 (COH), 61.03 (CH 2 O), 42.88 (CH 2 ), 14.21
+
4.09 (q, J = 7.2 Hz, 2H, OCH 2 ), 3.50 (s, 1H, OH), (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 245.14喠჋≸
2.67~2.54 (m, 2H, CH 2 ), 1.17 (t, J = 7.2 Hz, 3H, թ 245.12ȡ
13
CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į: 172.24 (O==C), 3-㓌ധ-3-(2-நॖധ)͆䚥Ά䚜喍11喎喟叱㞟⇦⟣
141.09 (Ar-C), 133.43 (Ar-C), 128.67 (Ar-C), 127.11 ➖ [28] 喑172.0 mg喑ϔ⢴ 86%ȡ HNMR (400 MHz,
1
(Ar-C), 69.63 (COH), 61.02 (CH 2 O), 43.26 (CH 2 ), CDCl 3 ), į: 7.30~7.20 (m, 1H, Ar-H), 6.98~6.96 (m,
+
14.14 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 228.10喠
2H, Ar-H), 5.37~5.36 (m, 1H, CHOH), 4.19 (q, J = 7.2
჋≸թ 228.06ȡ Hz, 2H, OCH 2 ), 2.93~2.79 (m, 2H, CH 2 ), 1.26 (d, J =
13
3-㓌ധ-3-(4-⅌㠜ധ)͆䚥Ά䚜喍7喎喟叱㞟⇦⟣➖ [29] 喑 7.2 Hz, 3H, CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į:
1
201.3 mg喑ϔ⢴ 95%ȡ HNMR (400 MHz, CDCl 3 ), į: 172.02 (O==C), 146.29 (Ar-C), 126.74 (Ar-C), 124.90
7.26~7.23 (m, 2H, Ar-H), 6.96~6.91 (m, 2H, Ar-H), (Ar-C), 123.67 (Ar-C), 66.57 (COH), 61.05 (CH 2 O),
5.02~4.99 (m, 1H, CHOH), 4.07 (q, J = 7.1 Hz, 2H, 43.15 (CH 2 ), 14.16 (CH 3 )ȡESI-MS, m/Z喟⤳䃧[M+H] +
OCH 2 ), 3.54 (s, 1H, OH), 2.67~2.53 (m, 2H, CH 2 ), թ 201.03喠჋≸թ 201.05ȡ
13
1.16 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR (101 MHz, 3-㓌ധ䓈䚥Ά䚜喍12喎喟叱㞟⇦⟣➖ [31] 喑158.0 mg喑
CDCl 3 ), į: 172.27 (O==C), 163.47 (Ar-C), 161.03 1
(Ar-C), 138.44 (Ar-C), 127.45 (Ar-C), 115.43 (Ar-C), ϔ⢴ 84%ȡ HNMR (400 MHz, CDCl 3 ), į: 4.21 (q, J =
115.22 (Ar-C), 69.67 (COH), 60.95 (CH 2 O), 43.42 7.2 Hz, 2H, OCH 2), 3.48 (s, 1H, CHOH), 2.83~2.55 (m,
+
(CH 2 ), 14.10 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 2H, CH 2 ), 1.43~1.23 (m, 11H, CH 2 CH 2 CH 2 CH 2 CH 3 ),
13
0.91~0.85 (m, 3H, CH 3 )ȡ CNMR (101 MHz, CDCl 3 ),
213.09喠჋≸թ 213.08ȡ
į: 203.89 (O==C), 167.00 (COH), 67.58 (CH 2 O),
3-㓌ധ-3-(2,5-ι⅌㠜ധ)͆䚥Ά䚜喍8喎喟叱㞟⇦ 61.56 (CH 2 ), 49.95 (CH 2 ), 49.64 (CH 2 ), 36.41 (CH 2 ),
1
⟣➖ [30] 喑211.6 mg喑ϔ⢴ 92%ȡ HNMR (400 MHz, 31.69 (CH 2 ), 25.11 (CH 2 ), 22.59 (CH 2 ), 14.09 (CH 3 )ȡ
CDCl 3 ), į: 7.24~7.10 (m, 1H, Ar-H), 6.91~26.85 (m, ESI-MS, m/Z喟[M+H] ⤳䃧թ 189.14喑჋≸թ 189.15ȡ
+
2H, Ar-H), 5.289~5.27 (m, 1H, CHOH), 4.09 (q, J =
7.2 Hz, 2H, OCH 2 ), 3.84 (br, 1H, OH), 2.71~2.51 (m, 3-㓌ധ-2,2-ι⅌-3-㠜ധ͆䚥Ά䚜喍13喎喟叱㞟⇦
1
13
2H, CH 2 ), 1.16 (t, J = 7.2 Hz, 3H, CH 3 )ȡ CNMR (101 ⟣➖ [32] 喑209.3 mg喑ϔ⢴ 91%ȡ HNMR (400 MHz,
MHz, CDCl 3 ), į: 172.19 (O==C), 160.16 (Ar-C), CDCl 3 ), į: 7.53~7.26 (m, 5H, Ar-H), 5.14~5.07 (m,
157.75 (Ar-C), 156.29 (Ar-C), 153.89 (Ar-C), 131.57 1H, CHOH), 4.24 (q, J = 7.2 Hz, 2H, OCH 2 ), 3.40 (br,
(Ar-C), 116.23 (Ar-C), 115.25 (Ar-C), 114.04 (Ar-C), 1H, OH), 1.23 (t, J = 7.2 Hz, 3H, CH 3 )ȡ CNMR (101
13