Water → 2-Difluoromethoxy-6-fluorobenzamide O-cyclopropylmethyl oxime

HRID 1840659노트

반응식

HRID 1840659 반응식
[H-].[Na+].[F:3][CH:4]([F:17])[O:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[C:7]=1[C:8](=[N:10][OH:11])[NH2:9].Br[CH2:19][CH:20]1[CH2:22][CH2:21]1.O>CN(C)C=O>[CH:20]1([CH2:19][O:11][N:10]=[C:8]([NH2:9])[C:7]2[C:12]([F:16])=[CH:13][CH:14]=[CH:15][C:6]=2[O:5][CH:4]([F:3])[F:17])[CH2:22][CH2:21]1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 81503BromomethylcyclopropaneHCID 545406342-Difluoromethoxy-6-fluorobenzamidoxime

생성물 1

HCID 867583662-Difluoromethoxy-6-fluorobenzamide O-cyclopropylmethyl oxime수율 52%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.4 g of 80% pure sodium hydride was added to a solution of 3.0 g of 2-difluoromethoxy-6-fluorobenzamidoxime in 30 ml of dimethylformamide (DMF) at 0 to 5° C. and the mixture was stirred at this temperature for 3 hours. 1.8 g of bromocyclopropylmethane were subsequently added at the same temperature, and stirring was subsequently continued for 2 hours at 5° C. and overnight at room temperature. The batch was stirred into 300 ml of water and extracted three times with in each case 70 ml of cyclohexane. After the cyclohexane had been evaporated, 1.9 g of the desired product were obtained.

후처리

  1. stirringstirring
  2. waitwas subsequently continued for 2 hours at 5° C. and overnight at room temperature
  3. extractionextracted three times with in each case 70 ml of cyclohexane
  4. customAfter the cyclohexane had been evaporated

출처 및 근거

ORD 기록
ord-e78294ea5fc14d3e9451f7cff9e47245
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06680402B2

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