Dimethylcarbamoyl Chloride → HCID 21434451、化合物

HRID 2398160ノート

反応式

HRID 2398160 の反応式
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].Cl.[CH2:8]1[C:14]2[CH:15]=[CH:16][C:17]([S:19]([NH2:22])(=[O:21])=[O:20])=[CH:18][C:13]=2[CH2:12][CH2:11][NH:10][CH2:9]1.C(N(CC)CC)C>CO>[CH3:1][N:2]([CH3:6])[C:3]([N:10]1[CH2:9][CH2:8][C:14]2[CH:15]=[CH:16][C:17]([S:19]([NH2:22])(=[O:20])=[O:21])=[CH:18][C:13]=2[CH2:12][CH2:11]1)=[O:4]

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 8471TriethylamineHCID 214344292,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide hydrochloride

生成物 1

HCID 21434451HCID 21434451、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

8.05 Ml. of dimethylcarbamoyl chloride are added dropwise while cooling at about 25° C. in the course of 3 minutes to a solution of 21.5 g. of 2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide hydrochloride and 24.5 ml. of triethylamine in 400 ml. of methanol and the mixture is subsequently stirred for a further 15 hours, during which a crystalline precipitate results. By evaporation of the solvent in vacuo and digestion and washing of the crystalline evaporation residue with water, there is obtained 3-dimethylcarbamoyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonamide, m.p. 192°-193° C.

後処理

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  2. customBy evaporation of the solvent in vacuo and digestion
  3. washwashing of the crystalline evaporation residue with water

出典と根拠

ORDレコード
ord-950a2e8bd6e841c8ac07a8fec5a9cf2d
出典データセット
uspto-grants-1977_05
特許番号
US04024128

反応ノート

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