Methanol → 1,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine Hydrochloride

HRID 1653707

반응식

HRID 1653707 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.[CH3:15]O>>[ClH:13].[CH3:15][O:9][C:8]([CH:6]1[CH2:7][NH:2][CH:3]=[N:4][CH2:5]1)=[O:10]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 703421841,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

생성물 1

HCID 199620591,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine Hydrochloride수율 60%

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (6.34 g, 38.5 mmol) was dissolved in anhydrous methanol (200 ml) with stirring, and thionyl chloride (2.74 ml, 38.5 mmol) was added dropwise. The resulting solution was refluxed with stirring for 18 hours, then evaporated in vacuo to white solids. The crude product was recrystallized from anhydrous methanol to yield 4.12 g (60%) white crystals, mp 160°-164° C. Calculated: C 40.34, H 6.21, N 15.69; found: C 40.17, H 6.41, N 15.73.

후처리

  1. temperatureThe resulting solution was refluxed
  2. stirringwith stirring for 18 hours
  3. customevaporated in vacuo to white solids
  4. customThe crude product was recrystallized from anhydrous methanol

출처 및 근거

ORD 기록
ord-4ab2bac8a4354d3d9ca040e5cec9d1c8
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

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