Water → HCID 178460720, 화합물

HRID 25291

반응식

HRID 25291 반응식
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]

참가 물질

6

반응물 4

HCID 962WaterHCID 7848Propyl mercaptanHCID 11430Potassium CarbonateHCID 178497552HCID 178497552, 화합물

생성물 1

HCID 178460720HCID 178460720, 화합물수율 18,004,832%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.52 g (5.0 nmol) 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.).

후처리

  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

출처 및 근거

ORD 기록
ord-dc0f6da8f3b045d2a4076930466059c1
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858639B2

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