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盐酸 → HCID 24857375,化合物

HRID 1908925
笔记
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反应方程式

HRID 1908925 反应方程式
[Cl:1][C:2]1[C:3]([CH3:39])=[C:4]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][O:24][C:25]3[CH:38]=[CH:37][C:28]4[C@H:29]([CH2:32][C:33]([O:35]C)=[O:34])[CH2:30][O:31][C:27]=4[CH:26]=3)[CH:18]=2)[C:5]([CH3:16])=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][S:12]([CH3:15])(=[O:14])=[O:13].CO.[OH-].[Na+].Cl>O.O1CCCC1>[Cl:1][C:2]1[C:3]([CH3:39])=[C:4]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][O:24][C:25]3[CH:38]=[CH:37][C:28]4[C@H:29]([CH2:32][C:33]([OH:35])=[O:34])[CH2:30][O:31][C:27]=4[CH:26]=3)[CH:18]=2)[C:5]([CH3:16])=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][CH2:11][S:12]([CH3:15])(=[O:13])=[O:14]
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 313盐酸HCID 887MethanolHCID 14798氢氧化钠HCID 57415031methyl [(3S)-6-({3'-chloro-2',6'-dimethyl-4'-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetate

产物 1

HCID 24857375HCID 24857375,化合物收率 63.4%

试剂、催化剂与溶剂 2

HCID 962
聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]
溶剂
HCID 8028四氢呋喃溶剂

反应条件

温度
50 °C

实验过程

To a solution of methyl [(3S)-6-({3′-chloro-2′,6′-dimethyl-4′-[3-(methylsulfonyl)propoxy]biphenyl-3-yl}methoxy)-2,3-dihydro-1-benzofuran-3-yl]acetate (0.676 g, 1.18 mmol) in a mixed solvent of methanol (2 mL) and tetrahydrofuran (4 mL) was added 2 M aqueous sodium hydroxide solution (1.2 mL), and the mixture was stirred at 50° C. for 2 hr. The reaction mixture was diluted with water, acidified with 1 M hydrochloric acid, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The precipitated crystals were recrystallized from diethyl ether-ethyl acetate to give the title compound (0.418 g, yield 63%) as colorless crystals.

后处理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe precipitated crystals were recrystallized from diethyl ether-ethyl acetate

来源与证据

ORD记录
ord-16a6f81a5b0f4fdeacd8d4c1e09545e3
来源数据集
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08598226B2

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