m-Chloroperbenzoic acid → HCID 87304579, 화합물

HRID 547809노트

반응식

HRID 547809 반응식
[F:1][C:2]([F:44])([F:43])[C:3]1[CH:4]=[C:5]([C:13]([CH3:42])([CH3:41])[C:14]([N:16]([C:18]2[C:19]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:20][C:21]([N:24]3[CH2:29][CH2:28][CH:27]([CH2:30][S:31][CH3:32])[CH2:26][CH2:25]3)=[N:22][CH:23]=2)[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.ClC1C=CC=C(C(OO)=[O:53])C=1.S([O-])(O)=O.[Na+]>ClCCl>[F:44][C:2]([F:1])([F:43])[C:3]1[CH:4]=[C:5]([C:13]([CH3:41])([CH3:42])[C:14]([N:16]([C:18]2[C:19]([C:33]3[CH:38]=[CH:37][C:36]([F:39])=[CH:35][C:34]=3[CH3:40])=[CH:20][C:21]([N:24]3[CH2:25][CH2:26][CH:27]([CH2:30][S:31]([CH3:32])=[O:53])[CH2:28][CH2:29]3)=[N:22][CH:23]=2)[CH3:17])=[O:15])[CH:6]=[C:7]([C:9]([F:10])([F:11])[F:12])[CH:8]=1

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 23665763Sodium BisulfiteHCID 86597695HCID 86597695, 화합물

생성물 1

HCID 87304579HCID 87304579, 화합물수율 89.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.25 g (0.39 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-[4′-(4-fluoro-2-methyl-phenyl)-4-methylsulfanylmethyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-5′-yl]-N-methyl-isobutyramide in 10 ml dichloromethane were added 95 mg (70%, 0.39 mmol) 3-chloroperbenzoic acid at 0° C. After completed addition, the reaction mixture was allowed to warm to room temperature and stirred over night. An aqueous solution of sodium hydrogensulfite was added and the mixture was stirred for 10 min. Basification with 1 N aqueous sodium hydroxide solution was followed by extraction with three portions of dichloromethane. The combined organic extracts were dried over sodium sulphate and concentrated. Flash column chromatography gave 0.23 g (89%) of the title compound as a white solid.

후처리

  1. additionaddition
  2. stirringthe mixture was stirred for 10 min
  3. extractionBasification with 1 N aqueous sodium hydroxide solution was followed by extraction with three portions of dichloromethane
  4. dry with materialThe combined organic extracts were dried over sodium sulphate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6b7e7e297d2741beba87cd70124ff2d2
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939533B2

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