Phenol → HCID 19934777、化合物

HRID 37102

反応式

HRID 37102 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=3[Cl:30])=[C:19]([CH2:31]Cl)[N:18]=[C:17]([N:33]3[CH2:38][CH2:37][O:36][CH2:35][CH2:34]3)[N:16]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[C:39]1([O-:45])[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.[Na+].C1(O)C=CC=CC=1.[OH-].[Na+]>CC(C)=O.O>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[C:26]([O:28][CH3:29])[CH:25]=[CH:24][C:23]=3[Cl:30])=[C:19]([CH2:31][O:45][C:39]3[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=3)[N:18]=[C:17]([N:33]3[CH2:34][CH2:35][O:36][CH2:37][CH2:38]3)[N:16]=2)(=[O:12])=[O:13])=[CH:7][CH:6]=1)([CH3:2])([CH3:4])[CH3:3]

参加物

7

反応物 4

HCID 996PhenolHCID 14798Sodium HydroxideHCID 4445035Phenolate SodiumHCID 199347554-tert-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-(morpholin-4-yl)-pyrimidin-4-yl]-benzenesulphonamide

生成物 1

HCID 19934777HCID 19934777、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒2 回HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

0.145 g of 4-tert.-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-6-chloromethyl-2-(morpholin-4-yl)-pyrimidin-4-yl]benzenesulphonamide (Example 4) in 3 ml of acetone was added to a sodium phenolate solution from 0,024 g of phenol and 0.06 g of NaOH in 2 ml of acetone and 1 ml of water. The reaction mixture was stirred at 80° C. under argon for 48 hours. Thereafter, the acetone was distilled off and the residue was partitioned between chloroform and water. The chloroform phase was washed with water, dried over sodium sulphate and the solvent was distilled off. The residue was chromatographed over silica gel with chloroform. 0.07 g of 4-tert.-butyl-N-[5-(2-chloro-5-methoxy-phenoxy)-2-morpholin-4-yl-6-phenoxymethyl-pyrimidin-4-yl]benzenesulphonamide, MS: M=639, was obtained.

後処理

  1. distillationThereafter, the acetone was distilled off
  2. customthe residue was partitioned between chloroform and water
  3. washThe chloroform phase was washed with water
  4. dry with materialdried over sodium sulphate
  5. distillationthe solvent was distilled off
  6. customThe residue was chromatographed over silica gel with chloroform

出典と根拠

ORDレコード
ord-d0aa28ba710c4f8cadc523ef1d3f73ae
出典データセット
uspto-grants-1995_05
特許番号
US05420129

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