3,4-Dichloroaniline → HCID 12862635, 화합물

HRID 65735

반응식

HRID 65735 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[Cl:9])[NH2:5].[CH:10]12[O:15][CH:11]1[CH2:12][CH2:13][CH2:14]2>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[Cl:9])[NH:5][C@@H:10]1[CH2:14][CH2:13][CH2:12][C@H:11]1[OH:15]

참가 물질

3

반응물 2

HCID 72573,4-DichloroanilineHCID 92446-Oxabicyclo[3.1.0]hexane

생성물 1

HCID 12862635HCID 12862635, 화합물수율 44%

실험 절차

A solution of 50.0 g. (0.31 mole) of 3,4-dichloroaniline in 100 ml. of cyclopentene oxide is refluxed for 7 days. The solution is evaporated and the residue triturated with 250 ml. of petroleum ether (b.p. 30°-60° C.) five times to remove unreacted 3,4-dichloroaniline. The residue is treated with excess ethereal hydrogen chloride and the resulting crude hydrochloride salt is recrystallized twice from a methanol/ethyl ether mixture to give trans-2-(3,4-dichloroanilino)cyclopentanol, 38.7 g. (44% yield), m.p. 167°-168° C. The ultraviolet, infrared and nuclear magnetic resonance spectra are consistent with the structure of this product.

후처리

  1. customThe solution is evaporated
  2. customthe residue triturated with 250 ml
  3. customof petroleum ether (b.p. 30°-60° C.) five times to remove unreacted 3,4-dichloroaniline
  4. additionThe residue is treated with excess ethereal hydrogen chloride
  5. customthe resulting crude hydrochloride salt is recrystallized twice from a methanol/ethyl ether mixture

출처 및 근거

ORD 기록
ord-427cf403d6b24e01bf077ce29d85e3cb
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128663

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