Hydrochloric Acid → 4-Dimethylamino-4-phenylcyclohexyl-acetic acid hydrochloride

HRID 908961노트

반응식

HRID 908961 반응식
[OH-].[K+].[ClH:3].C[O:5][C:6](=[O:23])[CH2:7][CH:8]1[CH2:13][CH2:12][C:11]([N:20]([CH3:22])[CH3:21])([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:10][CH2:9]1.Cl>C(O)C.CCOCC>[ClH:3].[CH3:22][N:20]([CH3:21])[C:11]1([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:12][CH2:13][CH:8]([CH2:7][C:6]([OH:23])=[O:5])[CH2:9][CH2:10]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 67386483(4-Dimethylamino-4-phenylcyclohexyl)acetic acid methyl ester hydrochloride

생성물 1

HCID 673861314-Dimethylamino-4-phenylcyclohexyl-acetic acid hydrochloride수율 95%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

1.7 M KOH (70.5 ml, 120 mmol) was added to a solution of (4-dimethylamino-4-phenylcyclohexyl)acetic acid methyl ester hydrochloride (1.79 g, 5.77 mmol) in ethanol (80 ml). The mixture was stirred at RT for 16 h. The reaction mixture was concentrated and the residue was taken up in water. The aqueous phase was extracted with ether, and 5.5 M hydrochloric acid (23.6 ml, 130 mmol) was added. After concentration of the aqueous phase, the residue was extracted with ethanol, the potassium chloride which remained was separated off and the filtrate was concentrated. The product was thereby obtained as a colourless, oily compound in a yield of 95% (1.62 g).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. additionwas added
  3. extractionAfter concentration of the aqueous phase, the residue was extracted with ethanol
  4. customthe potassium chloride which remained was separated off
  5. concentrationthe filtrate was concentrated
  6. customThe product was thereby obtained as a colourless, oily compound in a yield of 95% (1.62 g)

출처 및 근거

ORD 기록
ord-219a8f595b5a49e0bf4048331bc6de48
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017630B2

반응 노트

불러오는 중…