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Diisobutylaluminum hydride → [3-Phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]methanol

HRID 242873
ノート
印刷プレビュー

反応式

HRID 242873 の反応式
C([O:3][C:4]([C:6]1[N:7]([S:21]([C:24]2[CH:29]=[CH:28][C:27]([CH3:30])=[CH:26][CH:25]=2)(=[O:23])=[O:22])[C:8]2[C:13]([C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)=O)C.CC(C[AlH]CC(C)C)C>C1(C)C=CC=CC=1>[C:15]1([C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[N:7]([S:21]([C:24]3[CH:25]=[CH:26][C:27]([CH3:30])=[CH:28][CH:29]=3)(=[O:22])=[O:23])[C:6]=2[CH2:4][OH:3])[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
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

4

反応物 2

HCID 14487Diisobutylaluminum hydrideHCID 681575273-Phenyl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester

生成物 1

HCID 68156952[3-Phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]methanol収率 85.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
-78 °C

実験手順

To a stirred solution of 3-phenyl-1-(toluene-4-sulfonyl)-1H-indole-2-carboxylic acid ethyl ester (3.24 g, 7.72 mmol) in toluene (40 mL) at −78° C. and under a nitrogen atmosphere was added 1.0M DIBAL-H in toluene (23.2 mL, 23.2 mmol). The reaction mixture was stirred at −78° C. for 15 min then at −10° C. for 30 min. After re-cooling to −78° C., the reaction mixture was quenched with water (20 mL) then allowed to warm to RT. The mixture was partitioned between EtOAc and 1.0M HCl and the aqueous phase was extracted with additional EtOAc (×3). The combined organic fractions were washed with water, dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 30-100% DCM in pentane) affording the title compound as a white foam (2.49 g, 85%). LCMS (Method C): RT 4.77 min [M+Na]+ 400.1

後処理

  1. waitat −10° C. for 30 min
  2. temperatureAfter re-cooling to −78° C.
  3. customthe reaction mixture was quenched with water (20 mL)
  4. temperatureto warm to RT
  5. customThe mixture was partitioned between EtOAc and 1.0M HCl
  6. extractionthe aqueous phase was extracted with additional EtOAc (×3)
  7. washThe combined organic fractions were washed with water
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated in vacuo
  10. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 30-100% DCM in pentane)

出典と根拠

ORDレコード
ord-ea44d798d2ae4933b79b4d8b395a5f18
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08653089B2

反応ノート

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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