Ethanol → 1,4,5,6-Tetrahydro-5-ethoxycarbonylpyrimidine Hydrochloride

HRID 1653703

반응식

HRID 1653703 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.[CH2:15](O)[CH3:16]>>[ClH:13].[CH2:15]([O:9][C:8]([CH:6]1[CH2:7][NH:2][CH:3]=[N:4][CH2:5]1)=[O:10])[CH3:16]

참가 물질

4

반응물 3

HCID 702EthanolHCID 24386Thionyl ChlorideHCID 703421841,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride

생성물 1

HCID 200804501,4,5,6-Tetrahydro-5-ethoxycarbonylpyrimidine Hydrochloride수율 63%

실험 절차

1,4,5,6-Tetrahydropyrimidine-5-carboxylic acid hydrochloride (1.5 g, 9.12 mmol) was dissolved in absolute ethanol (40 ml) by heating. The thionyl chloride (1.1 g, 9.16 mmol) was added dropwise with stirring. The resulting solution was refluxed 20h and then evaporated to dryness in vacuo. The residue was taken up in absolute methanol (5 ml) and dry THF (10 ml) was added to induce crystallization, giving 1.1 g (63%) product as white crystals, mp 125°-127° C. 300 MHz nmr confirmed the product. Microanalysis calc.: C 43.64, H 6.75, N 14.55; found: C, 43.43, H 6.58, N 14.40.

후처리

  1. temperatureby heating
  2. customevaporated to dryness in vacuo
  3. additiondry THF (10 ml) was added
  4. customcrystallization

출처 및 근거

ORD 기록
ord-0a47118198fe430299b368f7293bee1b
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05403845

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