Triethylamine → 4D-083

HRID 1995343노트

반응식

HRID 1995343 반응식
[O:1]=[C:2]1[C:7]([C:8](O)=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1.C([N:19](CC)CC)C>ClCCl>[O:1]=[C:2]1[C:7]([C:8]([NH2:19])=[O:9])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 121489343-Oxo-6-phenyl-2,3-dihydropyridazine-4-carboxylic acid

생성물 1

HCID 14753284D-083

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxylic acid (1.92 g) ethyl chloroformate (1.1 g) and triethylamine (2.0 ml) in 50 ml of dichloromethane is allowed to stir at 25°-30° C. for 2 hours. Ammonia gas is then bubbled into the mixture for 15 minutes. Water (50 ml) is added and the dichloromethane is separated and concentrated on the rotary evaporator. The residue is chromatographed on silica gel with 2% methanol and chloroform to give 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxamide.

후처리

  1. customAmmonia gas is then bubbled into the mixture for 15 minutes
  2. additionWater (50 ml) is added
  3. customthe dichloromethane is separated
  4. concentrationconcentrated on the rotary evaporator
  5. customThe residue is chromatographed on silica gel with 2% methanol and chloroform

출처 및 근거

ORD 기록
ord-6d64a749ca7c42b59c90b51c53f1cb0b
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04404203

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