1,4-Dithian-2-one → HCID 21224734、化合物

HRID 612321ノート

反応式

HRID 612321 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-e8ca9205bba34ba8bcf423dda68c4f27
出典データセット
uspto-grants-1999_12
特許番号
US06004531

反応ノート

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