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

HRID 1598789
ノート
印刷プレビュー

反応式

HRID 1598789 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
60 °C

実験手順

(±)-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.

後処理

  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)

出典と根拠

ORDレコード
ord-049a10d333614782a47d81578727c7e7
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05739158

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート