Acetic Anhydride → 2-(Acetylamino)-3,6-dihydro-4-methyl-6-(3-nitrophenyl)-1,5(2H)-pyrimidinedicarboxylic acid, diethyl ester

HRID 1789580노트

반응식

HRID 1789580 반응식
[NH2:1][C:2]1[N:3]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:6]([CH3:8])[N:7]=1.[C:28](OC(=O)C)(=[O:30])[CH3:29]>ClCCl.N1C=CC=CC=1.C(OCC)(=O)C>[C:28]([NH:1][CH:2]1[NH:7][C:6]([CH3:8])=[C:5]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[N:3]1[C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:30])[CH3:29]

참가 물질

6

반응물 2

HCID 7918Acetic AnhydrideHCID 139572692-Amino-4-methyl-6-(3-nitrophenyl)-1,5(6H)-pyrimidinedicarboxylic acid, diethyl ester

생성물 1

HCID 139572712-(Acetylamino)-3,6-dihydro-4-methyl-6-(3-nitrophenyl)-1,5(2H)-pyrimidinedicarboxylic acid, diethyl ester

시약·촉매·용매 3

HCID 1049Pyridine용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 2-amino-4-methyl-6-(3-nitrophenyl)-1,5(6H)-pyrimidinedicarboxylic acid, diethyl ester (550 mg, 1.46 mmoles, see Example 2) in dichloromethane (5.0 ml) and pyridine (0.5 ml) was treated with acetic anhydride (0.3 ml) and the reaction was allowed to stir at room temperature for 1 hour. The colorless reaction mixture was diluted with ethyl acetate and was washed with 5% citric acid, sodium bicarbonate solution and brine. It was dried over anhydrous magnesium sulfate and evaporated to provide a colorless foam. Crystallization from ether-hexanes provided the title compound as a colorless solid, melting point 154.5°-156° C.

후처리

  1. washwas washed with 5% citric acid, sodium bicarbonate solution and brine
  2. dry with materialIt was dried over anhydrous magnesium sulfate
  3. customevaporated
  4. customto provide a colorless foam
  5. customCrystallization from ether-hexanes

출처 및 근거

ORD 기록
ord-99317e12e9e34e248ca2fd650b9d5d3c
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689414

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