Potassium Carbonate → HCID 86709374、化合物

HRID 2172191ノート

反応式

HRID 2172191 の反応式
C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]2[CH:27]=[CH:26][C:25]([CH:28]=O)=[CH:24][CH:23]=2)=[CH:18][CH:17]=1.[F:30][C:31]([F:47])([F:46])[O:32][C:33]1[CH:45]=[CH:44][C:36]([O:37][CH:38]2[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]2)=[CH:35][CH:34]=1.C(=O)([O-])[O-].[K+].[K+]>ClCCCl>[F:47][C:31]([F:30])([F:46])[O:32][C:33]1[CH:45]=[CH:44][C:36]([O:37][CH:38]2[CH2:39][CH2:40][N:41]([CH2:28][C:25]3[CH:24]=[CH:23][C:22]([C:19]4[CH:18]=[CH:17][C:16]([OH:15])=[CH:21][CH:20]=4)=[CH:27][CH:26]=3)[CH2:42][CH2:43]2)=[CH:35][CH:34]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 27592994-(4-hydroxyphenyl)benzaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 161154394-[4-(Trifluoromethoxy)phenoxy]piperidine

生成物 1

HCID 86709374HCID 86709374、化合物収率 68.4%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

Sodium triacetoxyborohydride (1.69 g) was added to a 1,2-dichloroethane solution (11 ml) of 4′-hydroxybiphenyl-4-carbaldehyde (1.13 g) and 4-(4-trifluoromethoxyphenoxy)piperidine (1.78 g) and stirred at room temperature overnight. A potassium carbonate aqueous solution was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer was washed with water, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:0→0:10) to afford the title compound as a yellow powder (1.73 g).

後処理

  1. extractionfollowed by extraction with dichloromethane
  2. washThe organic layer was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:0→0:10)

出典と根拠

ORDレコード
ord-4142d366029a4c22b1943b3f75290232
出典データセット
uspto-grants-2015_06
特許番号
US09051333B2

反応ノート

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