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Pyridine → 9H-fluoren-9-ylmethyl(2,4-dimethyl-5-{[(pyridin-3-ylmethyl)amino]sulfonyl}phenyl)carbamate

HRID 1802462
ノート
印刷プレビュー

反応式

HRID 1802462 の反応式
[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:30])[NH:17][C:18]3[CH:23]=[C:22]([S:24](Cl)(=[O:26])=[O:25])[C:21]([CH3:28])=[CH:20][C:19]=3[CH3:29])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[N:31]1[CH:36]=[CH:35][CH:34]=[C:33]([CH2:37][NH2:38])[CH:32]=1.N1C=CC=CC=1>C(Cl)Cl>[CH:1]1[C:13]2[CH:12]([CH2:14][O:15][C:16](=[O:30])[NH:17][C:18]3[CH:23]=[C:22]([S:24]([NH:38][CH2:37][C:33]4[CH:32]=[N:31][CH:36]=[CH:35][CH:34]=4)(=[O:26])=[O:25])[C:21]([CH3:28])=[CH:20][C:19]=3[CH3:29])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1
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 3

HCID 1049PyridineHCID 310183-PyridinemethanamineHCID 594360429h-Fluoren-9-ylmethyl[5-(chlorosulfonyl)-2,4-dimethylphenyl]carbamate

生成物 1

HCID 594361089H-fluoren-9-ylmethyl(2,4-dimethyl-5-{[(pyridin-3-ylmethyl)amino]sulfonyl}phenyl)carbamate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 9H-fluoren-9-ylmethyl[5-(chlorosulfonyl)-2,4-dimethylphenyl]carbamate (1.0 g, 2.3 mmol) in CH2Cl2 (23 mL) was added 1-pyridin-3-ylmethanamine (0.46 mL, 4.5 mmol) and pyridine (0.55 mL, 6.8 mmol). The bright yellow solution was then stirred at room temperature overnight and then quenched by the addition of sat. aq. NaHCO3 solution. The reaction was extracted with EtOAc and the organic extracted were dried over Na2SO4 and concentrated in vacuo. Purification by silica gel column chromatography (0-5% MeOH/DCM) afforded the title compound.

後処理

  1. customquenched by the addition of sat. aq. NaHCO3 solution
  2. extractionThe reaction was extracted with EtOAc
  3. extractionthe organic extracted
  4. dry with materialwere dried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customPurification by silica gel column chromatography (0-5% MeOH/DCM)

出典と根拠

ORDレコード
ord-e8510aed1e0d46bbb3cafaee6328fe98
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08349865B2

反応ノート

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