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Dichloromethane → HCID 67067838、化合物

HRID 1037405
ノート
印刷プレビュー

反応式

HRID 1037405 の反応式
[C:1]([O:5][C:6](=[O:36])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:27](=[O:28])[C:26]4[C:21](=[C:22](Br)[CH:23]=[CH:24][CH:25]=4)[O:20][C:19]=3[C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].ClCCl.C(N(CC)CC)C>CO>[CH3:1][O:5][C:6]([C:22]1[CH:23]=[CH:24][CH:25]=[C:26]2[C:21]=1[O:20][C:19]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)=[C:18]([C:15]1[CH:16]=[CH:17][C:12]([C:8]3([NH:7][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:36])[CH2:11][CH2:10][CH2:9]3)=[CH:13][CH:14]=1)[C:27]2=[O:28])=[O:36]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 67067700{1-[4-(8-Bromo-4-oxo-2-phenyl-4H-chromen-3-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester

生成物 1

HCID 67067838HCID 67067838、化合物収率 200.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

{1-[4-(8-Bromo-4-oxo-2-phenyl-4H-chromen-3-yl)-phenyl]-cyclobutyl}-carbamic acid tert-butyl ester (200 mg, 0.367 mmol), and [1,1′-bis(diphenylphosphino)-ferrocene]dischloropalladium(II) complex with dichloromethane (60 mg, 0.073 mmol) were loaded into a microwave vial. The vial was sealed and a solution of triethylamine (0.102 mL, 0.732 mmol) in MeOH (4 mL) was added. The vial was evacuated and flushed twice with argon, followed by carbon monoxide. The reaction mixture was heated conventionally at 50° C. under an atmosphere of carbon monoxide for 18 h. The reaction mixture was allowed to cool to RT and was concentrated in vacuo. The resultant residue was subjected to flash chromatography (SiO2, gradient 0 to 10% EtOAc in DCM) to give the title compound as a gum (193 mg, 100%). LCMS (Method G): RT=4.41 min, [M+H]+=526.

後処理

  1. customThe vial was sealed
  2. customThe vial was evacuated
  3. customflushed twice with argon
  4. temperatureto cool to RT
  5. concentrationwas concentrated in vacuo

出典と根拠

ORDレコード
ord-8dcb59a87b64480fbc8f541dc426c8b6
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08546376B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート