1,4-Dithian-2-one → HCID 21224734、化合物

HRID 1584537ノート

反応式

HRID 1584537 の反応式
[NH2:1][CH2:2][CH2:3][NH:4][C:5](=[O:15])[CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[N+:12]([O-:14])=[O:13].[O:16]=[C:17]1[CH2:22][S:21][CH2:20][CH2:19][S:18]1>CO.CC(C)=O>[SH:18][CH2:19][CH2:20][S:21][CH2:22][C:17]([NH:1][CH2:2][CH2:3][NH:4][C:5](=[O:15])[CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[N+:12]([O-:14])=[O:13])=[O:16]

参加物

5

反応物 2

HCID 5427241,4-Dithian-2-oneHCID 19593917HCID 19593917、化合物

生成物 1

HCID 21224734HCID 21224734、化合物収率 37.5%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 887Methanol溶媒

実験手順

N-(2-Aminoethyl)-(2-nitroimidazol-1-yl)acetamide (40 mg, 0.23 mmol) in methanol (0.5 cm3) was added to 2-oxo-1,4-dithiane (40 mg, 0.27 mmol) in acetone (0.2 cm3) under an atmosphere of dry nitrogen. The mixture was left at room temperature and monitored by n.m.r. spectroscopy until the reaction was complete. The bulk of the solvent was removed, and the resulting material purified by reverse phase h.p.l.c. using aqueous methanol as the eluant. The pure N-{2-[(2-mercaptoethylthio)acetylamino]ethyl}-(2-nitroimidazol-1-yl)acetamide (30 mg) was isolated as a pale yellow solid.

後処理

  1. waitThe mixture was left at room temperature
  2. customThe bulk of the solvent was removed
  3. customthe resulting material purified by reverse phase h.p.l.c

出典と根拠

ORDレコード
ord-bf984e4dbaa842449e4c033bcc94865f
出典データセット
uspto-grants-1999_08
特許番号
US05932707

反応ノート

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