Hydrochloric Acid → (4-Dimethylamino-4-phenylcyclohexylidene)acetic acid hydrochloride

HRID 908918

반응식

HRID 908918 반응식
[OH-].[K+].[ClH:3].C[O:5][C:6](=[O:23])[CH:7]=[C: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.CCOCC.Cl>C(O)C>[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][C:8](=[CH:7][C:6]([OH:23])=[O:5])[CH2:9][CH2:10]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14797Potassium HydroxideHCID 67386135(4-Dimethylamino-4-phenylcyclohexylidene)acetic acid methyl ester hydrochloride

생성물 1

HCID 67386703(4-Dimethylamino-4-phenylcyclohexylidene)acetic acid hydrochloride수율 98%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.7 M KOH (70.5 ml, 120 mmol) was added to a solution of (4-dimethylamino-4-phenylcyclohexylidene)acetic acid methyl ester hydrochloride (1.8 g, 5.8 mmol) in ethanol (200 ml) and the mixture was stirred at RT for 16 h. The reaction mixture was concentrated and the residue was taken up in water (40 ml). The aqueous phase was extracted by shaking with ether (2×40 ml), and 5.5 M hydrochloric acid (23.6 ml, 130 mmol) was added. After the aqueous phase had been concentrated, the residue was extracted with ethanol (2×40 ml), the potassium chloride which remained was separated off and the filtrate was concentrated. The hydrochloride of the acid was thereby obtained as a colourless solid in a yield of 98% (1.67 g).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. extractionThe aqueous phase was extracted
  3. additionwas added
  4. concentrationAfter the aqueous phase had been concentrated
  5. extractionthe residue was extracted with ethanol (2×40 ml)
  6. customthe potassium chloride which remained was separated off
  7. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-c1b813893309407887b16d63fe4d1012
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017630B2

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