Potassium Carbonate → HCID 20506316、化合物

HRID 2050288ノート

反応式

HRID 2050288 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]1.[F:13][C:14]1[CH:19]=[CH:18][C:17]([CH:20]([C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)Br)=[CH:16][CH:15]=1.C(=O)([O-])[O-].[K+].[K+]>O>[F:13][C:14]1[CH:15]=[CH:16][C:17]([CH:20]([C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)[O:1][CH:2]2[CH2:3][CH2:4][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:6][CH2:7]2)=[CH:18][CH:19]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 676651,1'-(Bromomethylene)bis(4-fluorobenzene)HCID 96394Ethyl 4-hydroxypiperidine-1-carboxylate

生成物 1

HCID 20506316HCID 20506316、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
140 °C

実験手順

A mixture of 21.5 parts of ethyl 4-hydroxy-1-piperidinecarboxylate, 35.2 parts of bis(4-fluorophenyl)bromomethane and 8.6 parts of potassium carbonate is stirred and heated in an oil-bath at 140° C. for 2 hours. The reaction mixture is allowed to cool to room temperature and water is added. The product is extracted with methylbenzene. The extract is washed successively with water, a diluted hydrochloric acid solution and a sodium bicarbonate solution, dried, filtered and evaporated. The forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure), yielding ethyl 4-[bis(4-fluorophenyl)methoxy]-1-piperidinecarboxylate as an oily residue.

後処理

  1. temperatureto cool to room temperature
  2. extractionThe product is extracted with methylbenzene
  3. washThe extract is washed successively with water
  4. dry with materiala diluted hydrochloric acid solution and a sodium bicarbonate solution, dried
  5. filtrationfiltered
  6. customevaporated
  7. distillationThe forerun is distilled off (bp. till 143° C. at 0.5-1 mm. pressure)

出典と根拠

ORDレコード
ord-599d899eb2434a94a0b908fe2ea8465d
出典データセット
uspto-grants-1980_04
特許番号
US04200641

反応ノート

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