Water → HCID 178460720、化合物

HRID 498953

反応式

HRID 498953 の反応式
Cl[C:2]1[CH:11]=[C:10]([C:12]2[C:13]([C:17]([F:20])([F:19])[F:18])=[N:14][NH:15][CH:16]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH2:21]([SH:24])[CH2:22][CH3:23].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH2:21]([S:24][C:2]1[CH:11]=[C:10]([C:12]2[C:13]([C:17]([F:20])([F:19])[F:18])=[N:14][NH:15][CH:16]=2)[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])[CH2:22][CH3:23]

参加物

6

反応物 4

HCID 962WaterHCID 7848Propyl mercaptanHCID 11430Potassium CarbonateHCID 178497552HCID 178497552、化合物

生成物 1

HCID 178460720HCID 178460720、化合物収率 18%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.52 g (5.0 mmol) of methyl 2-chloro-4-(3-trifluoromethylpyrazolyl)benzoate, 0.66 g (8.6 mmol) of 1-propanethiol and 0.83 g (6.0 mmol) of potassium carbonate were stirred in 5 ml of N,N-dimethylformamide at 60° C. for 24 hours. The resulting reaction mixture was poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by thin layer chromatography afforded 0.31 g of methyl 2-propylthio-4-(3-trifluoromethylpyrazolyl)benzoate as a white powder (m.p. 114-116° C.).

後処理

  1. customThe resulting reaction mixture
  2. extractionthe organic matters were extracted with 20 ml of ethyl acetate twice
  3. washwashed with 30 ml of water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe ethyl acetate was distilled off under reduced pressure
  6. customPurification of the residue by thin layer chromatography

出典と根拠

ORDレコード
ord-2c5671f66d5d46b186019dbd66010b51
出典データセット
uspto-grants-2010_08
特許番号
US07767626B2

関連ノート

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