Methylamine → HCID 178484963、化合物

HRID 1493186ノート

反応式

HRID 1493186 の反応式
CS[C:3](SC)=[N:4][S:5]([CH3:8])(=[O:7])=[O:6].[NH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:17]=[C:18]([CH2:22][N:23]([CH3:25])[CH3:24])[CH:19]=[CH:20][CH:21]=1.[CH3:26][NH2:27]>C(O)C>[CH3:8][S:5]([NH:4][C:3]([NH:27][CH3:26])=[N:11][CH2:12][CH2:13][CH2:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][N:23]([CH3:24])[CH3:25])[CH:17]=1)(=[O:7])=[O:6]

参加物

5

実験手順

N-Methanesulphonylcarbonimidodithioic acid dimethyl ester (3 g) and 3-[3-aminopropoxy]-N,N-dimethylbenzenemethanamine (2.5 g) were heated at reflux in ethanol for 4 hours. Methylamine was then added and the reflux continued for 11/2 hours. The solvent was removed and the residue was purified by column chromatography on silica with methanol to yield the title compound as a yellow gum (1.9 g). TLC methanol:0.88 ammonia (80:1) Rf 0.65. NMR (CDCl3) 2.85 m (1H); 2.9-3.3 m (3H); 3.0-4.3 brs (2H); 5.90 t (2H); 6.5 q (2H); 6.6 s (2H); 7.1 s (6H); 7.75 s (6H); 7.9 m (2H).

後処理

  1. custom2 hours
  2. customThe solvent was removed
  3. customthe residue was purified by column chromatography on silica with methanol

出典と根拠

ORDレコード
ord-1ed615ef274e4c2cac69a25aac722b7a
出典データセット
uspto-grants-1991_06
特許番号
US05021429

反応ノート

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