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

HRID 1606600노트

반응식

HRID 1606600 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 215439782-Butylamino-4-chloro-5-methylsulfonylbenzoic acid수율 34%

시약·촉매·용매 1

HCID 8076Glycol monoethyl ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a1d6f3fcb4104a4ebf5e99b9250a2aab
출처 데이터셋
uspto-grants-1976_04
특허 번호
US03953476

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