Page 238 - 《精细化工》2023年第4期

g924g ㇫㏳ࡃጒ FINE CHEMICALS す 40 ࢤ

OCH 2 ), 2.94 (dd, J = 137.4Ƞ15.9 Hz, 2H, CH 2 ), 1.53 (s, 27.22 (COHCH 3 ), 13.95 (CH 3 )ȡESI-MS, m/Z喟[M+H] +
13
3H, COHCH 3 ), 1.01 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR ⤳䃧թ 288.02喠჋≸թ 288.03ȡ
(101 MHz, CDCl 3 ), į: 173.03 (O==C), 160.33 (Ar-C), 3-㓌ധ-3-(4-⏡㠜ധ)̮䚥Ά䚜喍27喎喟ᬍ㞟⇦⟣
157.90 (Ar-C), 133.08 (Ar-C), 129.00 (Ar-C), 124.15 ➖ [28] 喑248.9 mg喑ϔ⢴ 87%ȡ HNMR (400 MHz,
1
(Ar-C), 115.91 (Ar-C), 71.52 (COH), 60.74 (CH 2 O), CDCl 3 ), į: 7.41~7.33 (m, 2H, Ar-H), 7.28~7.22 (m,
44.95 (CH 2 CO), 28.55 (COHCH 3 ), 13.93 (CH 3 )ȡ 2H, Ar-H), 4.39 (s, 1H, OH), 3.99 (q, J = 7.1, 2H,
+
ESI-MS, m/Z喟[M+H] ⤳䃧թ 227.10喠჋≸թ 227.11ȡ OCH 2 ), 2.90~2.65 (m, 2H, CH 2 ), 1.43 (s, 3H,
13
3-㓌ധ-3-(3-⅌㠜ധ)̮䚥Ά䚜喍23喎喟ᬍ㞟⇦⟣ COHCH 3 ), 1.07 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR
1
➖ [37] 喑206.4 mg喑ϔ⢴ 92%ȡHNMR (400 MHz, CDCl 3), (101 MHz, CDCl 3 ), į: 172.57 (O==C), 146.03 (Ar-C),
131.32 (Ar-C), 126.46 (Ar-C), 120.84 (Ar-C), 72.54
į: 7.21~7.20 (m, 1H, Ar-H), 7.15~7.07 (m, 2H, Ar-H),
6.85~6.82 (m, 1H, Ar-H), 4.41 (s, 1H, OH), 3.99 (q, (COH), 60.92 (CH 2 O), 46.13 (CH 2 CO), 30.61
+
J = 7.2 Hz, 2H, OCH 2 ), 2.92~2.66 (m, 2H, CH 2 ), 1.45 (COHCH 3 ), 14.03 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧
(s, 3H, COHCH 3 ), 1.07 (t, J = 7.2 Hz, 3H, CH 3 )ȡ թ 288.02喠჋≸թ 288.03ȡ
13 CNMR (101 MHz, CDCl 3 ), į: 172.58 (O==C), 3-㓌ധ-3-(2-㥅ധ)̮䚥Ά䚜喍28喎喟ᬍ㞟⇦⟣➖ [28] 喑
164.10 (Ar-C), 149.81 (Ar-C), 129.81 (Ar-C), 120.09 234.8 mg喑ϔ⢴ 91%ȡ HNMR (400 MHz, CDCl 3 ), į:
1
(Ar-C), 113.82 (Ar-C), 112.07 (Ar-C), 72.54 (COH), 8.80 (d, J = 8.6 Hz, 1H, Ar-H), 7.86~7.67 (m, 2H,
60.90 (CH 2 O), 46.16 (CH 2 CO), 30.56 (COHCH 3 ), Ar-H), 7.55~7.38 (m, 3H, Ar-H), 7.34~7.32 (m, 1H,
+
13.98 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧թ 227.10喠 Ar-H), 4.73 (s, 1H, OH), 4.14~3.98 (m, 2H, OCH 2 ),
჋≸թ 227.11ȡ 3.15~2.91 (m, 2H, CH 2 ), 1.83 (s, 3H, COHCH 3 ), 1.11
13
(t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR (101 MHz, CDCl 3 ),
3-㓌ധ-3-(4-⅌㠜ധ)̮䚥Ά䚜喍24喎喟ᬍ㞟⇦⟣
1
➖ [28] 喑212.4 mg喑ϔ⢴ 94%ȡ HNMR (400 MHz, į: 173.13 (O==C), 141.47 (Ar-C), 135.03 (Ar-C),
130.94 (Ar-C), 129.22 (Ar-C), 128.92 (Ar-C), 126.99
CDCl 3 ), į: 7.34~7.32 (m, 2H, Ar-H), 6.94~6.90 (m, (Ar-C), 125.51 (Ar-C), 125.28 (Ar-C), 124.78 (Ar-C),
2H, Ar-H), 4.38 (s, 1H, OH), 3.98 (q, J = 7.1 Hz, 2H, 122.85 (Ar-C), 74.63 (COH), 60.86 (CH 2 O), 46.26
OCH 2 ), 2.89~2.66 (m, 2H, CH 2 ), 1.44 (s, 3H, (CH 2 CO), 29.88 (COHCH 3 ), 14.11 (CH 3 )ȡESI-MS,
13
COHCH 3 ), 1.05 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR +
m/Z喟[M+H] ⤳䃧թ 259.13喠჋≸թ 259.11ȡ
(101 MHz, CDCl 3 ), į: 172.63 (O==C), 162.94 (Ar-C), 3-㓌ധ-3-(2-நॖധ)̮䚥Ά䚜喍29喎喟ᬍ㞟⇦⟣
160.51 (Ar-C), 142.70 (Ar-C), 142.67 (Ar-C), 126.31 [29] 1
(Ar-C), 115.04 (Ar-C), 72.50 (COH), 60.82 (CH 2 O), ➖ 喑186.2 mg喑ϔ⢴ 87%ȡ HNMR (400 MHz,
46.42 (CH 2 CO), 30.71 (COHCH 3 ), 13.98 (CH 3 )ȡ CDCl 3 ), į: 7.19~7.18 (m, 1H, Ar-H), 6.96~6.85 (m,
+
ESI-MS, m/Z喟[M+H] ⤳䃧թ 227.10喠჋≸թ 227.11ȡ 2H, Ar-H), 4.78 (s, 1H, OH), 4.12 (q, J = 7.1 Hz, 2H,
OCH 2 ), 3.01~2.79 (m, 2H, CH 2 ), 1.63 (s, 3H,
3-㓌ധ-3-(3-̶⅌⩟ധ㠜ധ)̮䚥Ά䚜喍25喎喟ᬍ COHCH 3 ), 1.20 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR
13
1
㞟⇦⟣➖ [33] 喑248.6 mg喑ϔ⢴ 90%ȡHNMR (400 MHz, (101 MHz, CDCl 3 ), į: 172.47 (O==C), 152.27 (Ar-C),
CDCl 3 ), į: 7.66 (s, 1H, Ar-H), 7.57 (d, J = 7.7 Hz, 1H, 126.73 (Ar-C), 124.04 (Ar-C), 122.02 (Ar-C), 71.90
Ar-H), 7.46~7.35 (m, 2H, Ar-H), 4.45 (s, 1H, OH), (COH), 60.97 (CH 2 O), 46.92 (CH 2 CO), 31.47
+
3.99 (q, J = 7.1 Hz, 2H, OCH 2 ), 2.95~2.70 (m, 2H, (COHCH 3 ), 14.06 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧
CH 2 ), 1.48 (s, 3H, COHCH 3 ), 1.06 (t, J = 7.1 Hz, 3H, թ 215.07喠჋≸թ 215.09ȡ
13
CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), į: 172.53 (O==C), 3-㓌ധ-3-(3-⩟ധ-4-ॎણധ)̮䚥Ά䚜喍30喎喟ᬍ
147.98 (Ar-C), 131.08 (Ar-C), 130.76 (Ar-C), 128.79 㞟⇦⟣➖喑182.9 mg喑ϔ⢴ 82%ȡ HNMR (400 MHz,
1
(Ar-C), 128.05 (Ar-C), 125.55 (Ar-C), 121.54 (CF 3 ), CDCl 3 ), į: 7.59~7.57 (m, 1H, Ar-H), 7.32~7.31 (m,
72.63 (COH), 60.99 (CH 2 O), 46.11 (CH 2 CO), 30.61 1H, Ar-H), 7.02~7.01 (m, 1H, Ar-H), 5.31 (s, 1H, OH),
+
(COHCH 3 ), 13.94 (CH 3 )ȡESI-MS, m/Z喟[M+H] ⤳䃧 4.04 (q, J = 7.1 Hz, 2H, OCH 2 ), 2.93~2.78 (m, 2H,
թ 277.10喠჋≸թ 277.11ȡ CH 2 ), 2.52 (s, 3H, Ar-CH 3 ), 1.56 (s, 3H, COHCH 3 ),
13
3-㓌ധ-3-(2-⏡㠜ധ)̮䚥Ά䚜喍26喎喟ᬍ㞟⇦⟣ 1.15 (t, J = 7.1 Hz, 3H, CH 3 )ȡ CNMR (101 MHz,
1
➖喑245.9 mg喑ϔ⢴ 86%ȡHNMR (400 MHz, CDCl 3 ), CDCl 3 ), į: 172.09 (O==C), 163.67 (Ar-C), 156.46
į: 7.81~7.80 (m, 1H, Ar-H), 7.49~7.47 (m, 1H, Ar-H), (Ar-C), 137.06 (Ar-C), 121.42 (Ar-C), 116.09 (Ar-C),
73.16 (COH), 60.34 (CH 2 O), 46.38 (CH 2 CO), 29.17
7.29~7.22 (m, 1H, Ar-H), 7.06~6.98 (m, 1H, Ar-H),
4.63 (s, 1H, OH), 3.96 (q, J = 7.2 Hz, 2H, OCH 2 ), (COHCH 3 ), 24.33 (Ar-CH 3 ), 14.09 (CH 3 )ȡESI-MS,
+
3.24~2.89 (m, 2H, CH 2 ), 1.67 (s, 3H, COHCH 3 ), 1.02 m/Z喟[M +H] ⤳䃧թ 224.12喠჋≸թ 223.12ȡ
13
(t, J = 7.2 Hz, 3H, CH 3 )ȡ CNMR (101 MHz, CDCl 3 ), 3-㓌ധ-3-(4-⩟㠜ധ)᜷䚥Ά䚜喍31喎喟ᬍ㞟⇦⟣
1
į: 172.94 (O==C), 144.40 (Ar-C), 134.92 (Ar-C), ➖ [28] 喑198.2 mg喑ϔ⢴ 84%ȡHNMR (400 MHz, CDCl 3),
128.82 (Ar-C), 128.24 (Ar-C), 127.53 (Ar-C), 119.67 į: 7.20 (d, J = 8.2 Hz, 2H, Ar-H), 7.05 (d, J = 7.9 Hz,
(Ar-C), 73.59 (COH), 60.78 (CH 2 O), 43.64 (CH 2 CO), 2H, Ar-H), 4.24 (s, 1H, OH), 3.95 (q, J = 7.4 Hz, 2H,