Phenol → HCID 19934777, 화합물

HRID 37102

반응식

HRID 37102 반응식
[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]

참가 물질

7

반응물 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

생성물 1

HCID 19934777HCID 19934777, 화합물

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0aa28ba710c4f8cadc523ef1d3f73ae
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420129

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