Acetic Acid → HCID 70546961, 화합물

HRID 615004

반응식

HRID 615004 반응식
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][CH:6]([C:10](=O)[CH3:11])[C:7](=O)[CH3:8])[CH3:2].[F:14][C:15]([F:25])([F:24])[C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([NH:22][NH2:23])[CH:17]=1.C(O)(=O)C>C(O)C>[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]1[C:10]([CH3:11])=[N:23][N:22]([C:18]2[CH:17]=[C:16]([C:15]([F:14])([F:25])[F:24])[CH:21]=[CH:20][CH:19]=2)[C:7]=1[CH3:8])[CH3:2]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 87820Ethyl 3-acetyl-4-oxopentanoateHCID 98650(3-(Trifluoromethyl)phenyl)hydrazine

생성물 1

HCID 70546961HCID 70546961, 화합물수율 85.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

14.9 grams 3,3-diacetyl-propionic acid-ethyl ester, 14.1 grams (α,α,α-trifluoro-m-tolyl)-hydrazine, 4.8 grams glacial acetic acid and 100 milliliters ethanol were mixed, and the mixture heated to boiling temperature under reflux for 1 hour. The reaction mixture was evaporated and the residue distilled to produce 22.3 grams of crude 3,5-dimethyl-1-(α,α,α-trifluoro-m-tolyl)-pyrazol-4-acetic acid ethyl ester. This ester was saponified as and worked up in accordance with the method described in Example (1b), using 4.0 grams sodium hydroxide as the base. The free acid was precipitated from the alkaline solution obtained in this manner by the addition of 2% acetic acid and of sufficient aqueous hydrochloric acid to complete the precipitation.

후처리

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 1 hour
  3. customThe reaction mixture was evaporated
  4. distillationthe residue distilled

출처 및 근거

ORD 기록
ord-312da3908e114012abd82082816a6a65
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04146721

연결된 노트

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