Methanesulfonamide → p-Hexadecylamino-N-(methylsulfonyl)benzamide

HRID 1980169

反応式

HRID 1980169 の反応式
Cl.[CH2:2]([NH:18][C:19]1[CH:27]=[CH:26][C:22]([C:23](Cl)=[O:24])=[CH:21][CH:20]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[CH3:28][S:29]([NH2:32])(=[O:31])=[O:30]>N1C=CC=CC=1>[CH2:2]([NH:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([NH:32][S:29]([CH3:28])(=[O:31])=[O:30])=[O:24])=[CH:21][CH:20]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]

参加物

4

反応物 2

HCID 72879MethanesulfonamideHCID 132553224-Hexadecylaminobenzoyl chloride hydrochloride

生成物 1

HCID 20437358p-Hexadecylamino-N-(methylsulfonyl)benzamide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 25.2 g. of 4-(hexadecylamino)benzoyl chloride hydrochloride and 5.8 g. of methanesulfonamide in 250 ml. of pyridine was stirred under reflux for 2 hours and then concentrated in vacuo. The residue was partitioned between water and diethyl ether; the aqueous layer acidified with 1N HCl, and the organic layer separated, dried (MgSO4), and evaporated. Crystallization of the residual white solid from 60% aqueous acetic acid followed by CH2Cl2 -hexane afforded the product as a white solid.

後処理

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between water and diethyl ether
  4. customthe organic layer separated
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customCrystallization of the residual white solid from 60% aqueous acetic acid

出典と根拠

ORDレコード
ord-2d2a8bdcad684177ba8902cfe50d99d7
出典データセット
uspto-grants-1984_11
特許番号
US04485105

関連ノート

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