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

HRID 1659572

반응식

HRID 1659572 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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°.

후처리

  1. customThe solvent was removed

출처 및 근거

ORD 기록
ord-1baaf465976a43f6b352682f54b4b04b
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04304780

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