Water → 4-[(4,5-Difluoro-2-methoxyphenoxy)methyl]-N-(triphenylmethyl)-1-piperidineethanamine

HRID 248347

反応式

HRID 248347 の反応式
Cl.[F:2][C:3]1[C:16]([F:17])=[CH:15][C:6]([O:7][CH2:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[C:5]([O:18][CH3:19])[CH:4]=1.Br[CH2:21][CH2:22][NH:23][C:24]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[F:2][C:3]1[C:16]([F:17])=[CH:15][C:6]([O:7][CH2:8][CH:9]2[CH2:14][CH2:13][N:12]([CH2:21][CH2:22][NH:23][C:24]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)[CH2:11][CH2:10]2)=[C:5]([O:18][CH3:19])[CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 15718287(2-Bromoethyl)tritylamineHCID 19763367HCID 19763367、化合物

生成物 1

HCID 197633854-[(4,5-Difluoro-2-methoxyphenoxy)methyl]-N-(triphenylmethyl)-1-piperidineethanamine収率 41.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

5.88 g (0.020 mol) of 4-[(4,5-difluoro-2-methoxyphenoxy)methyl]piperidine hydrochloride, 7.7 g (0.021 mol) of 2-bromo-N-(triphenylmethyl)ethylamine and 6.91 g (0.050 mol) of K2CO3 in 40 ml of DMF are reacted. The reaction mixture is heated to 90° C. for 8 hours. It is cooled to room temperature, poured into 500 ml of water and extracted 3 times with ethyl acetate. The organic phases are combined, washed with water, dried over MgSO4 and filtered, and the solvent is evaporated off under reduced pressure. The product is obtained in the form of an oil after chromatography. Yield: 41.5%.

後処理

  1. temperatureIt is cooled to room temperature
  2. extractionextracted 3 times with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated off under reduced pressure
  7. customThe product is obtained in the form of an oil after chromatography

出典と根拠

ORDレコード
ord-d32e64f01da745f7a4d7dbc8a579c938
出典データセット
uspto-grants-1993_05
特許番号
US05210086

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