Butylamine → 5-n-Butylsulphamyl-4-chloro-3-nitro-benzoic acid

HRID 1576733ノート

反応式

HRID 1576733 の反応式
[CH2:1]([NH2:5])[CH2:2][CH2:3][CH3:4].[OH-].[Na+].[Cl:8][C:9]1[C:17]([S:18](Cl)(=[O:20])=[O:19])=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][C:10]=1[N+:22]([O-:24])=[O:23]>O>[Cl:8][C:9]1[C:17]([S:18](=[O:19])(=[O:20])[NH:5][CH2:1][CH2:2][CH2:3][CH3:4])=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][C:10]=1[N+:22]([O-:24])=[O:23]

参加物

5

反応物 3

HCID 8007ButylamineHCID 14798Sodium HydroxideHCID 898924-Chloro-5-chlorosulfonyl-3-nitrobenzoic acid

生成物 1

HCID 215060165-n-Butylsulphamyl-4-chloro-3-nitro-benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The starting material is prepared as follows: To the stirred solution 7.3 g of n-butylamine, 8 g of sodium hydroxide in 200 ml of water, 30 g of 4-chloro-5-chlorosulfonyl-3-nitrobenzoic acid are added portionwise while keeping the temperature between 0° and 5°. After 1/2 hour the mixture is allowed to warm to room temperature for 2 hours. The supernatant solution is filtered, the filtrate combined with 25 ml of 2N of hydrochloric acid, the precipitate formed collected and recrystallized from aqueous ethanol, to yield the 4-chloro-3-nitro-5-n-butylsulfamoylbenzoic acid melting at 199°-201°.

後処理

  1. customThe starting material is prepared
  2. customthe temperature between 0° and 5°
  3. filtrationThe supernatant solution is filtered
  4. customthe precipitate formed
  5. customcollected
  6. customrecrystallized from aqueous ethanol

出典と根拠

ORDレコード
ord-8ba24dcecc424f3695465a00432f1018
出典データセット
uspto-grants-1976_09
特許番号
US03982018

反応ノート

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