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Dimethylformamide dimethyl acetal → N,N-Dimethyl-N'-(6-hydroxybenzothiazole-2-sulfonyl)formamidine

HRID 2164613
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HRID 2164613 반응식
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[OH:9][C:10]1[CH:22]=[CH:21][C:13]2[N:14]=[C:15]([S:17]([NH2:20])(=[O:19])=[O:18])[S:16][C:12]=2[CH:11]=1>C(#N)C>[CH3:6][N:4]([CH3:5])[CH:3]=[N:20][S:17]([C:15]1[S:16][C:12]2[CH:11]=[C:10]([OH:9])[CH:22]=[CH:21][C:13]=2[N:14]=1)(=[O:18])=[O:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 68521296-Hydroxy-1,3-benzothiazole-2-sulfonamide

생성물 1

HCID 54375873N,N-Dimethyl-N'-(6-hydroxybenzothiazole-2-sulfonyl)formamidine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

N,N-Dimethylformamide dimethyl acetal (1.5 mL, 11.3 mmol) was added to a partial suspension of 6-hydroxybenzothiazole-2-sulfonamide (2.3 gm, 10 mmol) in acetonitrile (20 mL) to give an immediate solution. After stirring at room temperature for 1 hour, the reaction mixture was cooled and the crystalline product which formed (1.95 gm) was collected m.p. 195°-198° C. Evaporation of the reaction solvent and dissolution of the residue in ethyl acetate/acetonitrile which was washed with water, dried (Na2SO4) and evaporated yielded an additional 0.6 gm from methylene chloride.

후처리

  1. customto give an immediate solution
  2. temperaturethe reaction mixture was cooled
  3. customthe crystalline product which formed (1.95 gm)
  4. customwas collected m.p. 195°-198° C
  5. customEvaporation of the reaction solvent and dissolution of the residue in ethyl acetate/acetonitrile which
  6. washwas washed with water
  7. dry with materialdried (Na2SO4)
  8. customevaporated
  9. customyielded an additional 0.6 gm from methylene chloride

출처 및 근거

ORD 기록
ord-994f65202ef24baf9fabeca17d9d6211
출처 데이터셋
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04505923

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