Diisopropylethylamine → 4,6-Dimethoxy-2-(alpha-fluorobenzyl) pyrimidine

HRID 1440962노트

반응식

HRID 1440962 반응식
Cl.Cl.[C:3](=[NH:11])([O:9][CH3:10])[CH2:4][C:5](=[NH:8])[O:6][CH3:7].C(N(C(C)C)C(C)C)C.[F:21][CH:22]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:23](Cl)=O>ClCCl>[CH3:7][O:6][C:5]1[CH:4]=[C:3]([O:9][CH3:10])[N:11]=[C:23]([CH:22]([F:21])[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[N:8]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 12896693Dimethyl malonimidate dihydrochlorideHCID 149495282-Fluoro-2-phenylacetyl chloride

생성물 1

HCID 541012184,6-Dimethoxy-2-(alpha-fluorobenzyl) pyrimidine수율 103.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

Dimethyl malonimidate dihydrochloride (11.0 g) was suspended in dichloromethane (100 ml) at -40° C. Ethyl diisopropylamine (38.9 ml) was added dropwise over 15 minutes at -40° C., followed by 2-fluoro-2-phenylacetyl chloride (11.0 g) in dichloromethane (15 ml) over 10 minutes at -40° C. The reaction mixture was allowed to warm to room temperature and stand overnight. It was then diluted further with dichloromethane, washed with ammonium chloride solution, then with water, and was dried over magnesium sulfate. The dichloromethane solution was evaporated to dryness to give 13.9 g of the desired product.

후처리

  1. washwashed with ammonium chloride solution
  2. dry with materialwith water, and was dried over magnesium sulfate
  3. customThe dichloromethane solution was evaporated to dryness

출처 및 근거

ORD 기록
ord-6138cea4710c432493891253a750fc80
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05502028

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