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

HRID 259534
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HRID 259534 반응식
[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
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참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 10176082Aluminum HydroxideHCID 21226445Aluminium lithium hydride2회HCID 470031361,2-Benzisothiazol-3(2H)-one, 5,6-dimethoxy-, 1,1-dioxide

생성물 1

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

시약·촉매·용매 3

HCID 313
Hydrochloric Acid
용매
HCID 962Water용매
HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-09dd617fbedb4af9bd22c2ea4c78bb3e
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04038407

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