461-28-9 → HCID 59547781、化合物

HRID 2177075ノート

反応式

HRID 2177075 の反応式
[C:1]([O:5][C:6](=[O:27])[NH:7][CH:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([CH2:18][NH2:19])=[CH:13][CH:14]=2)[CH:9]1[CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)([CH3:4])([CH3:3])[CH3:2].[F:28][CH2:29][CH2:30][CH2:31][S:32](Cl)(=[O:34])=[O:33]>ClCCl.CN(C)C1C=CN=CC=1>[C:1]([O:5][C:6](=[O:27])[NH:7][CH:8]1[CH2:17][CH2:16][C:15]2[C:10](=[CH:11][C:12]([CH2:18][NH:19][S:32]([CH2:31][CH2:30][CH2:29][F:28])(=[O:34])=[O:33])=[CH:13][CH:14]=2)[CH:9]1[CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 21114841461-28-9HCID 57471193Tert-butyl [7-(aminomethyl)-1-benzyl-1,2,3,4-tetrahydronaphthalen-2-yl]carbamate

生成物 1

HCID 59547781HCID 59547781、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

Tert-butyl[7-(aminomethyl)-1-benzyl-1,2,3,4-tetrahydronaphthalen-2-yl]carbamate (32 mg, 0.87 mmol) was dissolved in dichloromethane (15 mL) and 4-dimethylaminopyridine (12 mg, 0.096 mmol) and 3-fluoropropane-1-sulfonyl chloride (14 mg, 0.087 mmol) were added. The reaction mixture was stirred at room temperature over night. The dichloromethane solution of the crude product was washed successively with 1N aqueous hydrochloric acid and aqueous NaHCO3 solution, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by flash chromatography (dichloromethane, methanol, silica gel). Yield: 9.3 mg (0.019 mmol, 22%).

後処理

  1. washThe dichloromethane solution of the crude product was washed successively with 1N aqueous hydrochloric acid and aqueous NaHCO3 solution
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated in vacuo
  4. customThe crude product was purified by flash chromatography (dichloromethane, methanol, silica gel)

出典と根拠

ORDレコード
ord-d1bd3a3ef1f84c7f9919decb70bbfc0e
出典データセット
uspto-grants-2015_06
特許番号
US09067871B2

反応ノート

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