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2-Chlorobenzenesulfonyl chloride → 2-Chloro-N-[4-(7,8-dimethoxy-1-oxo-2,2a,4,5-tetrahydro-1H-3-aza-acenaphthylen-3-yl)-butyl]-benzenesulfonamide hydrochloride

HRID 1988124
ノート
印刷プレビュー

反応式

HRID 1988124 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8](Cl)(=[O:10])=[O:9].Cl.Cl.[NH2:14][CH2:15][CH2:16][CH2:17][CH2:18][N:19]1[CH2:29][CH2:28][C:27]2[C:30]3[CH:20]1[CH2:21][C:22](=[O:35])[C:23]=3[C:24]([O:33][CH3:34])=[C:25]([O:31][CH3:32])[CH:26]=2>C(Cl)Cl>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8]([NH:14][CH2:15][CH2:16][CH2:17][CH2:18][N:19]1[CH2:29][CH2:28][C:27]2[C:30]3[CH:20]1[CH2:21][C:22](=[O:35])[C:23]=3[C:24]([O:33][CH3:34])=[C:25]([O:31][CH3:32])[CH:26]=2)(=[O:10])=[O:9]
参加物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 761872-Chlorobenzenesulfonyl chlorideHCID 673585823-(4-Amino-butyl)-7,8-dimethoxy-2a,3,4,5-tetrahydro-2H-3-aza-acenaphthylen-1-one dihydro-chloride

生成物 1

HCID 441239432-Chloro-N-[4-(7,8-dimethoxy-1-oxo-2,2a,4,5-tetrahydro-1H-3-aza-acenaphthylen-3-yl)-butyl]-benzenesulfonamide hydrochloride収率 119%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-Chlorobenzenesulfonyl chloride (92.4 mg, 0.44 mmol) was added to a solution of 3-(4-Amino-butyl)-7,8-dimethoxy-2a,3,4,5-tetrahydro-2H-3-aza-acenaphthylen-1-one dihydro-chloride (150 mg, 0.40 mmol) and NN′-diisopropylethylamine (0.400 ml) in CH2Cl2 (20 mL) and the mixture was stirred overnight at room temperature. The resulting solution was washed with water (3×20 mL), dried over Na2SO4 and evaporated to dryness. The free base was dissolved in ethyl acetate (2 ml) and A 2.8 M solution of hydrogen chloride in ethanol was then added. The product was crystallized and collected by filtration, and vacuum dried to give a pale brown solid (135 mg, 66%).

後処理

  1. washThe resulting solution was washed with water (3×20 mL)
  2. dry with materialdried over Na2SO4
  3. customevaporated to dryness
  4. dissolutionThe free base was dissolved in ethyl acetate (2 ml)
  5. additionA 2.8 M solution of hydrogen chloride in ethanol was then added
  6. customThe product was crystallized
  7. filtrationcollected by filtration, and vacuum
  8. customdried

出典と根拠

ORDレコード
ord-cbf001c4f4e54891a77d2280ca5044cd
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07553965B2

反応ノート

読み込み中…

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