Oxalic acid dihydrate → N,N-dimethyl-3-[3-[(1-methylthio-2-nitroethenyl)amino]propoxy]benzenemethanamine

HRID 1659572ノート

反応式

HRID 1659572 の反応式
[NH2:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]([CH2:12][N:13]([CH3:15])[CH3:14])[CH:9]=[CH:10][CH:11]=1.[CH3:16][S:17][CH:18](SC)[CH2:19][N+:20]([O-:22])=[O:21].O.O.C(O)(=O)C(O)=O>O1CCCC1>[CH3:15][N:13]([CH3:14])[CH2:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([O:5][CH2:4][CH2:3][CH2:2][NH:1][C:18]([S:17][CH3:16])=[CH:19][N+:20]([O-:22])=[O:21])[CH:7]=1

参加物

5

反応物 3

HCID 61373Oxalic acid dihydrateHCID 123722641,1-Bis(methylsulfanyl)-2-nitroethaneHCID 129139503-(3-Aminopropoxy)-N,N-dimethylbenzenemethanamine

生成物 1

HCID 70538402N,N-dimethyl-3-[3-[(1-methylthio-2-nitroethenyl)amino]propoxy]benzenemethanamine収率 64%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-(3-Aminopropoxy)-N,N-dimethylbenzenemethanamine (10 g) and 1,1-bis-(methylthio)-2-nitroethane (16 g) were heated under reflux in tetrahydrofuran for 19 hours. Oxalic acid dihydrate (1.3 g) was added and the resulting precipitate was discarded. The solvent was removed to leave the title compound as a crystalline solid (10 g) m.p. 59°-63°.

後処理

  1. customThe solvent was removed

出典と根拠

ORDレコード
ord-1baaf465976a43f6b352682f54b4b04b
出典データセット
uspto-grants-1981_12
特許番号
US04304780

反応ノート

読み込み中…