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Potassium Carbonate → HCID 59381939、化合物

HRID 2354572
ノート
印刷プレビュー

反応式

HRID 2354572 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[N:19](S(C2C=CC=CC=2)(=O)=O)[CH:18]=[C:17]3[C:32]#[N:33])[CH:10]([CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])([O-])=O.[K+].[K+]>CO.O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[C:16]3[C:20](=[CH:21][CH:22]=2)[NH:19][CH:18]=[C:17]3[C:32]#[N:33])[CH:10]([CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 59381925HCID 59381925、化合物

生成物 1

HCID 59381939HCID 59381939、化合物収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a suspension of 4-(1-benzenesulfonyl-3-cyano-1H-indol-5-yl)-3-benzyl-piperazine-1-carboxylic acid tert-butyl ester (0.37 g, 0.7 mmol) in 10 mL MeOH was added K2CO3 (0.27 g, 2.0 mmol) in 2 mL H2O. The reaction mixture was stirred for 30 minutes and then solution was concentrated under reduced pressure and extracted with EtOAc. The combine organic layers were dried over MgSO4, filtered, and concentrated under reduced pressure. Purification via flash chromatography (25% EtOAc in hexane) afforded 3-benzyl-4-(3-cyano-1H-indol-5-yl)-piperazine-1-carboxylic acid tert-butyl ester (0.23 g, 85%) as a white foam; MS (M+H)=417.

後処理

  1. concentrationsolution was concentrated under reduced pressure
  2. extractionextracted with EtOAc
  3. dry with materialThe combine organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification via flash chromatography (25% EtOAc in hexane)

出典と根拠

ORDレコード
ord-fb2403272c7047e5b1fbe7a9620d98fd
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07754721B2

反応ノート

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