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1,1-Dimethylhydrazine → HCID 13849570, 화합물

HRID 2413517
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HRID 2413517 반응식
[NH2:1][S:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[S:11](Cl)(=[O:13])=[O:12])(=[O:4])=[O:3].[CH3:15][N:16]([CH3:18])[NH2:17]>O1CCCC1>[CH3:15][N:16]([CH3:18])[NH:17][S:11]([C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[S:2]([NH2:1])(=[O:4])=[O:3])(=[O:13])=[O:12]
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참가 물질

4

반응물 2

HCID 59761,1-DimethylhydrazineHCID 138495692-Sulfamoylbenzene-1-sulfonyl chloride

생성물 1

HCID 13849570HCID 13849570, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 1.28 g of 2-(aminosulfonyl)benzenesulfonyl chloride in 12 mL of dry tetrahydrofuran (THF) was cooled to -65° C. and a solution of 0.88 mL of 1,1-dimethylhydrazine in 12 mL of dry THF added dropwise. The resulting mixture was allowed to warm to room temperature, filtered, and the filtrate concentrated in vacuo. The solid residue was partitioned between water and ethyl acetate, the organic phase was separated, washed with water, washed with brine, dried (MgSO4), concentrated in vacuo, and the residue triturated with 1-chlorobutane to provide 1.07 g of the subject compound, m.p. 122°-124° C. (dec).

후처리

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated in vacuo
  3. customThe solid residue was partitioned between water and ethyl acetate
  4. customthe organic phase was separated
  5. washwashed with water
  6. washwashed with brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo
  9. customthe residue triturated with 1-chlorobutane

출처 및 근거

ORD 기록
ord-b051e3627c944d079077d038f15ce969
출처 데이터셋
uspto-grants-1988_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04718938

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