Hydrogen Peroxide → 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid

HRID 1627745노트

반응식

HRID 1627745 반응식
[F:1][CH:2]([F:11])[C:3]1[C:7]([CH:8]=[O:9])=[CH:6][N:5]([CH3:10])[N:4]=1.[OH-:12].[Na+].OO>O>[F:11][CH:2]([F:1])[C:3]1[C:7]([C:8]([OH:12])=[O:9])=[CH:6][N:5]([CH3:10])[N:4]=1

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 533020643-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde2회

생성물 1

HCID 189830083-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid수율 83%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
42.5 °C

실험 절차

A 3-neck 250 ml round bottomed flask was fitted with a magnetic stirrer and thermometer. Water (130 g), the product of example 1 (compound of formula IX) (6.50 g) and aqueous sodium hydroxide (8.17 g) were charged to the reactor, and the resulting solution heated to 40-45° C. A 35% hydrogen peroxide solution (39 g) was added over 1 hr, and the mixture then stirred at 40-45° C. for 0.5 hr [83% yield of desired product (compound of formula XI)−quantitative HPLC]. The pH of the reaction mass was adjusted to 2.5 by addition of 36% aqueous hydrochloric acid solution. The resulting precipitate was isolated by filtration and washed with water. Drying (60° C., 10 mbar) gave the desired product (XI) as pale yellow, free-flowing powder [69% yield of desired product−quantitative HPLC].

후처리

  1. customA 3-neck 250 ml round bottomed flask was fitted with a magnetic stirrer

출처 및 근거

ORD 기록
ord-b52c8f1e1beb4b7395421d11cbfb77b2
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785657B2

반응 노트

불러오는 중…