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Ammonia → cis-N-methyl-2-(1-pyrrolidinyl)cyclohexylamine

HRID 1598789
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반응식

HRID 1598789 반응식
[N:1]1([C@H:6]2[CH2:11][CH2:10][CH2:9][CH2:8][C@H:7]2[N:12](C(OC(C)(C)C)=O)[CH3:13])[CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.N>>[N:1]1([C@H:6]2[CH2:11][CH2:10][CH2:9][CH2:8][C@H:7]2[NH:12][CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5]1
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참가 물질

4

반응물 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 86745978(+/-)-cis-2-Pyrrolidinyl-N-t-butyloxycarbonyl-N-methylcyclohexylamine

생성물 1

HCID 13377466cis-N-methyl-2-(1-pyrrolidinyl)cyclohexylamine

반응 조건

온도
60 °C

실험 절차

(±)-cis-2-Pyrrolidinyl-N-t-butyloxycarbonyl-N-methylcyclohexylamine (247 gm) was slowly added to 6M hydrochloric acid at 60° C. with vigorous stirring. The solution was stirred an additional 5 minutes at 60° C. and poured onto ice (200 gm). Excess concentrated aqueous ammonia was added and the mixture was extracted with methylene chloride. The combined extracts were dried (Na2SO4) and the solvent removed on a rotary evaporator. The residue was distilled (78° C. at 0.3 mm Hg) to give the product as a colorless oil.

후처리

  1. additionpoured onto ice (200 gm)
  2. extractionthe mixture was extracted with methylene chloride
  3. dry with materialThe combined extracts were dried (Na2SO4)
  4. customthe solvent removed on a rotary evaporator
  5. distillationThe residue was distilled (78° C. at 0.3 mm Hg)

출처 및 근거

ORD 기록
ord-049a10d333614782a47d81578727c7e7
출처 데이터셋
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05739158

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