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Acetic Anhydride → N-[6-(3-Fluoro-benzenesulfonylamino)-1,2,3,4-tetrahydro-naphthalen-1-ylmethyl]-acetamide

HRID 492088
ノート
印刷プレビュー

反応式

HRID 492088 の反応式
[NH2:1][CH2:2][CH:3]1[CH2:12][CH2:11][CH2:10][C:9]2[CH:8]=[C:7]([NH:13][S:14]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[CH:18]=3)(=[O:16])=[O:15])[CH:6]=[CH:5][C:4]1=2.[C:24](OC(=O)C)(=[O:26])[CH3:25]>N1C=CC=CC=1.O>[F:23][C:19]1[CH:18]=[C:17]([S:14]([NH:13][C:7]2[CH:8]=[C:9]3[C:4](=[CH:5][CH:6]=2)[CH:3]([CH2:2][NH:1][C:24](=[O:26])[CH3:25])[CH2:12][CH2:11][CH2:10]3)(=[O:16])=[O:15])[CH:22]=[CH:21][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

5

反応物 2

HCID 7918Acetic AnhydrideHCID 57678960N-(5-aminomethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-3-fluoro-benzenesulfonamide

生成物 1

HCID 57678959N-[6-(3-Fluoro-benzenesulfonylamino)-1,2,3,4-tetrahydro-naphthalen-1-ylmethyl]-acetamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1049Pyridine溶媒

反応条件

温度
23 °C

実験手順

To a solution of 0.18 grams (0.538 mmoles) N-(5-aminomethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-3-fluoro-benzenesulfonamide in 25 mL pyridine was added 0.052 grams (0.511 mmole) acetic anhydride. The reaction mixture was stirred at 23° C. for 4 hours. The mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed with 0.5M hydrochloric acid, water, and saturated aqueous sodium chloride. The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure. N-[6-(3-Fluoro-benzenesulfonylamino)-1,2,3,4-tetrahydro-naphthalen-1-ylmethyl]-acetamide was obtained as a crystalline solid from ethyl acetate/ethyl ether, 0.18 grams (89%), m.p. 136-137° C., M+H=377.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with 0.5M hydrochloric acid, water, and saturated aqueous sodium chloride
  3. dry with materialThe organic phase was dried (magnesium sulfate)
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-58c13340c6cc47568021d2890df78cff
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07531577B2

反応ノート

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