Methane → Isopropyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride

HRID 1653705

반응식

HRID 1653705 반응식
Cl.[NH:2]1[CH2:7][CH:6]([C:8]([OH:10])=[O:9])[CH2:5][N:4]=[CH:3]1.S(Cl)([Cl:13])=O.C.[CH3:16][CH:17](O)[CH3:18]>>[ClH:13].[NH:4]1[CH2:5][CH:6]([C:8]([O:10][CH:17]([CH3:18])[CH3:16])=[O:9])[CH2:7][N:2]=[CH:3]1

참가 물질

5

반응물 4

HCID 297MethaneHCID 3776IsopropanolHCID 24386Thionyl ChlorideHCID 703421841,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

생성물 1

HCID 20080421Isopropyl 1,4,5,6-Tetrahydropyrimidine-5-carboxylate Hydrochloride수율 84%

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.0 g, 6.08 mmol) was suspended in 2-propanol (50 ml) and thionyl chloride (0.76 g, 6.39 mmol) was added dropwise. The resulting mixture was refluxed 24h. The pink solution was treated with charcoal and then reduced in volume to 15 ml by evaporating unreacted alcohol. By allowing the solution to stand overnight, white crystals (1.08 g, 84%) were obtained in three crops, mp 170° C. 300 MHz nmr confirmed product. Microanalysis calc.: C 46.49, H 7.26, N 13.56, found: C 46.49, H 7.25, N 13.64.

후처리

  1. temperatureThe resulting mixture was refluxed 24h
  2. customby evaporating unreacted alcohol

출처 및 근거

ORD 기록
ord-c2c5fed39ba44851add36118fd640225
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

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