Butylamine → 2-Butylamino-4-chloro-5-methylsulfonylbenzoic acid

HRID 1606600ノート

反応式

HRID 1606600 の反応式
Cl[C:2]1[CH:10]=[C:9]([Cl:11])[C:8]([S:12]([CH3:15])(=[O:14])=[O:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:16]([NH2:20])[CH2:17][CH2:18][CH3:19]>CCOCCO>[CH2:16]([NH:20][C:2]1[CH:10]=[C:9]([Cl:11])[C:8]([S:12]([CH3:15])(=[O:14])=[O:13])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5])[CH2:17][CH2:18][CH3:19]

参加物

4

反応物 2

HCID 8007ButylamineHCID 221013652,4-Dichloro-5-methanesulfonylbenzoic acid

生成物 1

HCID 215439782-Butylamino-4-chloro-5-methylsulfonylbenzoic acid収率 34%

試薬・触媒・溶媒 1

HCID 8076Glycol monoethyl ether溶媒

実験手順

A mixture of 2,4-dichloro-5-methylsulfonylbenzoic acid (6.0 g.; 0.0224 mole), butylamine (9 ml.) and ethyl cellosolve (20 ml.) is heated at reflux in a nitrogen atmosphere for 5 hours. The solvent is distilled at reduced pressure and the residue is dissolved in water (75 ml.) then treated with dilute hydrochloric acid which causes the product to precipitate. After recrystallization from butyl chloride there is collected 2.3 g. (34% yield) of 2-butylamino-4-chloro-5-methylsulfonylbenzoic acid, m.p. 187°-9° C.

後処理

  1. temperatureis heated
  2. temperatureat reflux in a nitrogen atmosphere for 5 hours
  3. distillationThe solvent is distilled at reduced pressure
  4. dissolutionthe residue is dissolved in water (75 ml.)
  5. additionthen treated with dilute hydrochloric acid which
  6. customto precipitate
  7. customAfter recrystallization from butyl chloride
  8. customthere is collected 2.3 g

出典と根拠

ORDレコード
ord-a1d6f3fcb4104a4ebf5e99b9250a2aab
出典データセット
uspto-grants-1976_04
特許番号
US03953476

反応ノート

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