Water → HCID 131723643、化合物

HRID 1018588ノート

反応式

HRID 1018588 の反応式
[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]

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 10184617HCID 10184617、化合物HCID 438334963-Picolyl chloride hydrochloride

生成物 1

HCID 131723643HCID 131723643、化合物収率 93%

実験手順

(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+).

後処理

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

出典と根拠

ORDレコード
ord-1923056442544e5893602bb2419e4a43
出典データセット
uspto-grants-2002_11
特許番号
US06482829B2

反応ノート

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