Hydroxylamine → HCID 178523962、化合物
反応式
C([O:4][CH2:5][C:6]1[N:19]=[C:9]2[N:10]=[C:11]([C:15](OC)=[O:16])[CH:12]=[C:13]([SH:14])[N:8]2[N:7]=1)(=O)C.[NH2:20][OH:21]>CO>[OH:21][NH:20][C:15]([C:11]1[CH:12]=[C:13]([SH:14])[N:8]2[N:7]=[C:6]([CH2:5][OH:4])[N:19]=[C:9]2[N:10]=1)=[O:16]参加物
4
実験手順
Methyl 2-(acetoxymethyl)-7-mercapto-s-triazolo[1,5-a]pyrimidine-5-carboxylate (80 mg) (0.28 mmol) are dissolved in 3 ml of absolute methanol. 188 mg (5.7 mmol) of hydroxylamine are added within 4 days while stirring. The product is precipitated (pH 6) with 3N aqueous hydrochloric acid, filtered off under suction and washed with methanol. After crystallization from methanol there are obtained 50 mg of N-hydroxy-2-(hydroxymethyl)-7-mercapto-s-triazolo[1,5-a]pyrimidine-5-carboxamide as a yellow powder.
後処理
- customThe product is precipitated (pH 6) with 3N aqueous hydrochloric acid
- filtrationfiltered off under suction
- washwashed with methanol
- customAfter crystallization from methanol
出典と根拠
- ORDレコード
- ord-404092c8a41343869b131343689daef4
- 出典データセット
- uspto-grants-1995_08
- 特許番号
- US05438052
反応ノート
読み込み中…