Hydrochloric Acid → 3-Chloro-2-[1-(4-chlorophenyl)-1-methoxycarbonyl-methyl]-5-trifluoromethylpyridine

HRID 1250144노트

반응식

HRID 1250144 반응식
Cl.[C:2]([CH:5]([C:13]1[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][N:14]=1)[C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=1)(=[O:4])N.[CH3:24][OH:25]>>[Cl:19][C:18]1[C:13]([CH:5]([C:6]2[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][CH:7]=2)[C:2]([O:25][CH3:24])=[O:4])=[N:14][CH:15]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:17]=1

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 37609312-(4-Chlorophenyl)-2-[3-chloro-5-(trifluoromethyl)-2-pyridinyl]acetamide

생성물 1

HCID 183272733-Chloro-2-[1-(4-chlorophenyl)-1-methoxycarbonyl-methyl]-5-trifluoromethylpyridine

실험 절차

Hydrogen chloride gas was introduced into a solution of 3.0 g of 2-[1-carbamoyl-1-(4-chlorophenyl)methyl]-3-chloro-5-trifluoromethylpyridine (prepared by the method of Example 3) in 100 ml of anhydrous methanol for 5 hours. The mixture was subsequently stirred for another 16 hours and excess hydrogen chloride was removed by passing nitrogen through the mixture. The methanol was separated off and the crude product was purified by silica gel chromatography (eluent: cyclohexane/tert-butyl methyl ether 50:1). Yield: 1.3 g (42%) of colorless crystals; mp.: 103-104° C.

후처리

  1. customexcess hydrogen chloride was removed
  2. customThe methanol was separated off
  3. customthe crude product was purified by silica gel chromatography (eluent: cyclohexane/tert-butyl methyl ether 50:1)

출처 및 근거

ORD 기록
ord-dc956572f5a94612908079865a8cb83a
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06337305B1

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