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三苯基膦 → HCID 10169000,化合物

HRID 1069221
笔记
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反应方程式

HRID 1069221 反应方程式
CCOC(/N=N/C(OCC)=O)=O.[Br:13][C:14]1[CH:19]=[C:18]([C:20]2[C:32]3[C:31]([CH3:33])=[C:30]([CH3:34])[S:29][C:28]=3[C:27]([Br:35])=[C:26]3[C:21]=2[CH:22]=[CH:23][CH:24]=[CH:25]3)[CH:17]=[C:16]([Br:36])[C:15]=1[OH:37].O[C@@H:39]([CH2:44][C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1)[C:40]([O:42][CH3:43])=[O:41].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CCOCC.C1C=CC=CC=1>[CH3:43][O:42][C:40](=[O:41])[C@H:39]([O:37][C:15]1[C:16]([Br:36])=[CH:17][C:18]([C:20]2[C:32]3[C:31]([CH3:33])=[C:30]([CH3:34])[S:29][C:28]=3[C:27]([Br:35])=[C:26]3[C:21]=2[CH:22]=[CH:23][CH:24]=[CH:25]3)=[CH:19][C:14]=1[Br:13])[CH2:44][C:45]1[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=1
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

7

反应物 4

HCID 11776三苯基膦HCID 5289077L-3-苯基乳酸甲酯HCID 5462977偶氮二甲酸二乙酯HCID 9893519HCID 9893519,化合物

产物 1

HCID 10169000HCID 10169000,化合物收率 97.4%

试剂、催化剂与溶剂 2

HCID 241Benzene溶剂
HCID 3283
乙醚
溶剂

反应条件

温度
80 °C

实验过程

Diethylazodicarboxylate (0.262 mL, 1.67 mmol) was added dropwise to a stirred, room temperature solution of 2,6dibromo-4-(9-bromo-2,3-dimethyl-naphtho[2,3-b]thiophen-4-yl)-phenol (0.60 g, 1.11 mmol), and (S)-2-hydroxy-3-phenylpropionic acid, methyl ester (0.300 g, 1.67 mmol), triphenylphosphine (0.437 g, 1.67 mmol) and benzene (5 mL) and the solution was heated in an 80° C. oil bath for 6 h. Upon cooling to room temperature, the reaction mixture was diluted with ether and silica gel (30 mL) was added. The reaction mixture was concentrated and the silica adsorbate was flash chromatographed (95:5 petroleum ether:ethyl acetate) to provide the title compound as a white solid (0.76 g, 97%): mp 174-175° C.: NMR (DMSO-d6); δ8.21 (ddd, J=8,1,1 Hz, 1H), 7.74 (d, J=2 Hz, 1H), 7.73 (d, J=2 Hz, 1H),7.67 (ddd, J=8, 6, 1 Hz, 1H), 7.53 (ddd, J=8, 7, 1 Hz, 1H), 7,43 (d, J=8 Hz, 1H), 7.35-7.24 (m, 5H), 5.11 (dd, J=7, 6 Hz, 1H), 3.61 (s, 3H), 3.43 (dd, 13, 6 Hz, 1H), 3.40 (dd, 13, 7 Hz, 1H), 2.44 (d, J=1 Hz, 3H), 1.60 (d, J=1 Hz, 3H); MS (+FAB): 3 bromine isotope pattern 700(20%), 702 (70%), 704 (75%), 706 (25%); Anal. Calc. for C30H23Br3O3S: C, 51.23; H, 3.30; N, 0.00. Found: C, 51.52; H, 3.36; N, 0.12.

后处理

  1. temperatureUpon cooling to room temperature
  2. additionwas added
  3. concentrationThe reaction mixture was concentrated
  4. customchromatographed (95:5 petroleum ether:ethyl acetate)

来源与证据

ORD记录
ord-cd5ece204b414a70810f9fb27837c435
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06251936B1

反应笔记

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本页导航参与物反应条件实验过程后处理来源与证据反应笔记