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Hydrochloric Acid → HCID 178479248, 화합물

HRID 1657568
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HRID 1657568 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C@H:10]2[CH2:15][CH2:14][C@H:13]([NH:16]C(=O)C)[CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[ClH:20]>CO>[ClH:20].[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([C@H:10]2[CH2:15][CH2:14][C@H:13]([NH2:16])[CH2:12][CH2:11]2)=[CH:8][CH:9]=1)([O-:3])=[O:2]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178474954HCID 178474954, 화합물

생성물 1

HCID 178479248HCID 178479248, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 5.25 g. of trans N-[4-(p-nitrophenyl)cyclohexyl]acetamide (prepared as in Example 81) in 50 ml. of hydrochloric acid and 50 ml. of methanol is heated at reflux for about 72 hours. The bulk of the methanol is then removed under vacuum and the residue dissolved in 100 ml. of hot water. The solution is then made strongly basic and extracted with ether and the organic layer then evaporated to dryness to give trans 4-(p-nitrophenyl)cyclohexylamine (I). The residue is dissolved in a small amount of ether which is then treated with 4.9 g. hydrochloric acid in ether to give 4.78 g. (99% yield) of trans N-4-(p-nitrophenyl)cyclohexylamine hydrochloride (I). The analytical sample has a melting point of 293° to 294° C.

후처리

  1. temperatureat reflux for about 72 hours
  2. customThe bulk of the methanol is then removed under vacuum
  3. dissolutionthe residue dissolved in 100 ml
  4. extractionextracted with ether
  5. customthe organic layer then evaporated to dryness

출처 및 근거

ORD 기록
ord-f0dc86981aef4c6eb023fcdac96640fb
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03960961

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