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

HRID 1653705

反応式

HRID 1653705 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.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

参加物

5

反応物 4

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

生成物 1

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

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-c2c5fed39ba44851add36118fd640225
出典データセット
uspto-grants-1995_04
特許番号
US05403845

関連ノート

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