Water → HCID 67170155、化合物

HRID 2170844ノート

反応式

HRID 2170844 の反応式
CS(O[CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)(=O)=O.[F:19][C:20]([F:30])([F:29])[O:21][C:22]1[CH:23]=[C:24]([SH:28])[CH:25]=[CH:26][CH:27]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[F:30][C:20]([F:19])([F:29])[O:21][C:22]1[CH:23]=[C:24]([S:28][CH:6]2[CH2:7][CH2:8][N:9]([C:12]([O:14][C:15]([CH3:16])([CH3:17])[CH3:18])=[O:13])[CH2:10][CH2:11]2)[CH:25]=[CH:26][CH:27]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 27773573-(Trifluoromethoxy)thiophenolHCID 41848691-(tert-Butoxycarbonyl)-4-(methanesulfonyloxy)piperidine

生成物 1

HCID 67170155HCID 67170155、化合物収率 74.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of tert-butyl 4-((methylsulfonyl)oxy)piperidine-1-carboxylate (1.34 g, 4.79 mmol), 3-(trifluoromethoxy)benzenethiol (1.12 g, 5.75 mmol) and potassium carbonate (1.99 g, 14.4 mmol) in N,N-dimethylformamide (50 mL) at 90° C. for 20 hours. The mixture was poured into water (200 mL) and extracted with ethyl acetate (200 mL). The organic layer was washed with water (200 mL) and dried over sodium sulfate. After removal of the solvent, the residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (20:1) to give 1.34 g (74%) of the title compound as colorless oil.

後処理

  1. extractionextracted with ethyl acetate (200 mL)
  2. washThe organic layer was washed with water (200 mL)
  3. dry with materialdried over sodium sulfate
  4. customAfter removal of the solvent
  5. customthe residue was purified by column chromatography on silica gel eluting with n-hexane/ethyl acetate (20:1)

出典と根拠

ORDレコード
ord-0e765156a3454814b3acb12e41e6553c
出典データセット
uspto-grants-2015_06
特許番号
US09051296B2

反応ノート

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