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

HRID 1653703

反応式

HRID 1653703 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.[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]

参加物

4

反応物 3

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

生成物 1

HCID 200804501,4,5,6-Tetrahydro-5-ethoxycarbonylpyrimidine Hydrochloride収率 63%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0a47118198fe430299b368f7293bee1b
出典データセット
uspto-grants-1995_04
特許番号
US05403845

関連ノート

読み込み中…