Water → HCID 131723643, 화합물

HRID 1018588노트

반응식

HRID 1018588 반응식
[F:1][C:2]([F:34])([F:33])[C:3]1[CH:4]=[C:5]([CH:26]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:28]=1)[C:6]([N:8]1[CH2:25][CH2:24][C:11]2([N:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH:14]([CH3:22])[NH:13][C:12]2=[O:23])[CH2:10][CH2:9]1)=[O:7].[H-].[Na+].[Cl-].ClC[C:40]1[CH:41]=[NH+:42][CH:43]=[CH:44][CH:45]=1.O.[CH3:47]N(C)C=O>>[F:34][C:2]([F:1])([F:33])[C:3]1[CH:4]=[C:5]([CH:26]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:28]=1)[C:6]([N:8]1[CH2:9][CH2:10][C:11]2([N:15]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:14]([CH3:47])([CH3:22])[N:13]([C:40]3[CH:41]=[N:42][CH:43]=[CH:44][CH:45]=3)[C:12]2=[O:23])[CH2:24][CH2:25]1)=[O:7]

참가 물질

6

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 10184617HCID 10184617, 화합물HCID 438334963-Picolyl chloride hydrochloride

생성물 1

HCID 131723643HCID 131723643, 화합물수율 93%

실험 절차

(rac)-8-(3,5-Bis-trifluoromethyl-benzoyl)-2-methyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one (200 mg, 0.41 mmol) was dissolved in dimethyl formamide (10 mL) and sodium hydride (40 mg, 60% in mineral oil, 1 mmol) and 3-chloromethyl pyridinium chloride (82 mg, 0.5 mmol) were added and stirred at room temperature overnight. Water (30 mL) was added and the reaction mixture extacted with ethyl actetate. The organic phases were pooled, dried with MgSO4 and the solvent was evaporated. The residue was purified by chromatography on silica gel (ethyl acetate) to yield the desired product (219 mg, 93%), MS: m/e=577.0 (M+H+).

후처리

  1. dry with materialdried with MgSO4
  2. customthe solvent was evaporated
  3. customThe residue was purified by chromatography on silica gel (ethyl acetate)

출처 및 근거

ORD 기록
ord-1923056442544e5893602bb2419e4a43
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06482829B2

반응 노트

불러오는 중…