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Ethyl Acetate → 5,6-Dimethoxy-1,2-benzisothiazoline-1,1-dioxide

HRID 259534
ノート
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反応式

HRID 259534 の反応式
[CH3:1][O:2][C:3]1[C:4]([O:15][CH3:16])=[CH:5][C:6]2[S:10](=[O:12])(=[O:11])[NH:9][C:8](=O)[C:7]=2[CH:14]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.[OH-].[Al+3].[OH-].[OH-]>O1CCCC1.O.Cl>[CH3:1][O:2][C:3]1[C:4]([O:15][CH3:16])=[CH:5][C:6]2[S:10](=[O:12])(=[O:11])[N:9]=[CH:8][C:7]=2[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 8857Ethyl AcetateHCID 10176082Aluminum HydroxideHCID 21226445Aluminium lithium hydride2 回HCID 470031361,2-Benzisothiazol-3(2H)-one, 5,6-dimethoxy-, 1,1-dioxide

生成物 1

HCID 681175355,6-Dimethoxy-1,2-benzisothiazoline-1,1-dioxide

試薬・触媒・溶媒 3

HCID 313
Hydrochloric Acid
溶媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

7 gm (288 millimols) of the compound obtained in step (c) were refluxed for 2 hours with 3.3 gm (865 millimols) of lithium aluminum hydride in 400 ml of tetrahydrofuran. After cooling, the excess lithium aluminum hydride was decomposed by addition of ethyl acetate, the mixture was diluted with water, and subsequently 2 N hydrochloric acid was added until the aluminum hydroxide precipitate was dissolved. The reaction solution now extracted with ethyl acetate, and the organic phase was washed with water, dried and evaporated in vacuo. The residue was digested in ether, and the desired compound was suction-filtered off.

後処理

  1. temperatureAfter cooling
  2. dissolutionwas dissolved
  3. extractionThe reaction solution now extracted with ethyl acetate
  4. washthe organic phase was washed with water
  5. customdried
  6. customevaporated in vacuo
  7. filtrationthe desired compound was suction-filtered off

出典と根拠

ORDレコード
ord-09dd617fbedb4af9bd22c2ea4c78bb3e
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04038407

反応ノート

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