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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Formaldehyde → 2-Cyclohexen-1-one, 5,5-dimethyl-3-(2-chlorophenylamino)-2-piperidinomethyl-, monohydrochloride

HRID 461674
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HRID 461674 반응식
[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[NH:4][C:5]1[CH2:10][C:9]([CH3:12])([CH3:11])[CH2:8][C:7](=[O:13])[CH:6]=1.[CH2:18]=O.Cl.[NH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1>CO.C(O)(=O)C>[ClH:1].[Cl:1][C:2]1[CH:17]=[CH:16][CH:15]=[CH:14][C:3]=1[NH:4][C:5]1[CH2:10][C:9]([CH3:12])([CH3:11])[CH2:8][C:7](=[O:13])[C:6]=1[CH2:18][N:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1
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참가 물질

6

반응물 3

HCID 712FormaldehydeHCID 2723721Piperidine, hydrochloride (1:1)HCID 13002203HCID 13002203, 화합물

생성물 1

HCID 30399422-Cyclohexen-1-one, 5,5-dimethyl-3-(2-chlorophenylamino)-2-piperidinomethyl-, monohydrochloride

시약·촉매·용매 2

HCID 176Acetic Acid촉매HCID 887Methanol
용매

실험 절차

12.5 Parts of 3-(2-chloroanilino)-5,5-dimethyl-2-cyclohexen-1-one is dissolved in 3o volume parts of methanol under warming and, then, to the resulting solution are added 4.5 parts of a 37 weight % aqueous solution of formaldehyde, 6.05 parts of piperidine hydrochloride and 2 drops of glacial acetic acid. The whole mixture is allowed to stand at room temperature for 1 hour, whereupon a yellow, clear solution is obtained. The methanol is distilled off under reduced pressure, and a small amount of isopropyl ether is added to the resulting residue, followed by cooling, whereupon colorless crystals separate. The crystals are collected by filtration and recrystallized from acetone. The procedure yields colorless prisms of 3-(2-chloroanilino)-5,5-dimethyl-2-piperidinomethyl-2-cyclohexen-1-one hydrochloride. Melting point: 105°-106° C.

후처리

  1. temperatureunder warming
  2. customwhereupon a yellow, clear solution is obtained
  3. distillationThe methanol is distilled off under reduced pressure
  4. additiona small amount of isopropyl ether is added to the resulting residue
  5. temperatureby cooling, whereupon colorless crystals
  6. customseparate
  7. filtrationThe crystals are collected by filtration
  8. customrecrystallized from acetone

출처 및 근거

ORD 기록
ord-bb0aff482f9442e99eabb0b12a075675
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04064133

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