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

HRID 1653707

反応式

HRID 1653707 の反応式
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]

参加物

4

反応物 3

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

生成物 1

HCID 199620591,4,5,6-Tetrahydro-5-methoxycarbonylpyrimidine Hydrochloride収率 60%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ab2bac8a4354d3d9ca040e5cec9d1c8
出典データセット
uspto-grants-1995_04
特許番号
US05403845

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