Acetic Acid → HCID 18694317, 화합물

HRID 1870870노트

반응식

HRID 1870870 반응식
[CH3:1][N:2]1[CH:7]2[CH2:8][CH2:9][CH:3]1[CH2:4][C:5]([C:11]1[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=1)(O)[CH2:6]2.C(O)(=O)C.Cl.[C:26]([OH:32])(=[O:31])[CH2:27][C:28]([OH:30])=[O:29]>C(O)C>[C:26]([OH:32])(=[O:31])[CH2:27][C:28]([OH:30])=[O:29].[CH3:1][N:2]1[CH:7]2[CH2:8][CH2:9][CH:3]1[CH:4]=[C:5]([C:11]1[CH:12]=[CH:13][C:14]([C:17]([F:18])([F:19])[F:20])=[CH:15][CH:16]=1)[CH2:6]2

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 867Malonic AcidHCID 4350948-methyl-3-(4-trifluoromethylphenyl)-8-azabicyclo[3.2.1]octan-3-ol

생성물 1

HCID 18694317HCID 18694317, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

The title compound was prepared from 8-methyl-3-(4-trifluoromethylphenyl)-8-azabicyclo[3.2.1]octan-3-ol (5 g, 17.5 mmol), glacial acetic acid (16 mL) and concentrated hydrochloric acid (16 mL). The free base of the title compound was dissolved in ethanol (96%) and added malonic acid (1.17 g, 11.2 mmol) in ethanol (96%), the solution was concentrated to dryness, and the residue was trituated in diethyl ether, the title compound precipitated as powder and was isolated by filtration. Yield 3.9 g (60%), m.p. 106.7-107.8° C.

후처리

  1. concentrationthe solution was concentrated to dryness
  2. customthe title compound precipitated as powder
  3. customwas isolated by filtration

출처 및 근거

ORD 기록
ord-b74aa689f1ce4dfea61c4b07e1db4967
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06100275

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