Acetic Acid → HCID 18694317、化合物

HRID 1870870ノート

反応式

HRID 1870870 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 18694317HCID 18694317、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b74aa689f1ce4dfea61c4b07e1db4967
出典データセット
uspto-grants-2000_08
特許番号
US06100275

反応ノート

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