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Potassium Carbonate → HCID 22033113、化合物

HRID 1792293
ノート
印刷プレビュー

反応式

HRID 1792293 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH2:15]Br)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[N:17]1([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.CN(C=O)C>[C:1]([C:5]1[CH:6]=[C:7]([CH2:15][N:20]2[CH2:19][CH2:18][N:17]([C:23]([O:25][C:26]([CH3:29])([CH3:28])[CH3:27])=[O:24])[CH2:22][CH2:21]2)[CH:8]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 44475071-(Bromomethyl)-3,5-di-tert-butylbenzene

生成物 1

HCID 22033113HCID 22033113、化合物収率 56.1%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6228Dimethylformamide
溶媒

実験手順

3,5-Bis(t-butyl)-1-(bromomethyl)benzene (170 mg, 0.60 mmol), t-butyl piperazine carboxylate (102 mg, 0.55 mmol) and potassium carbonate (151 mg, 1.10 mmol) were dissolved in a solvent mixture of acetone (2 ml) and DMF (0.2 ml), and the mixture was stirred overnight while heated under reflux. The reaction mixture was extracted with ethyl acetate, dried over sodium sulfate, and then the filtrate was evaporated under reduced pressure. The concentrate was subjected to silica gel column chromatography (n-hexane:ethyl acetate=4:1) to give 120 mg (yield: 56%) of the title compound as a white solid.

後処理

  1. temperaturewhile heated
  2. temperatureunder reflux
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. dry with materialdried over sodium sulfate
  5. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-0c4bcea7fa9f4f4fbae5be5b7622ef17
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07074819B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート