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

HRID 2164613
ノート
印刷プレビュー

反応式

HRID 2164613 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-994f65202ef24baf9fabeca17d9d6211
出典データセット
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04505923

反応ノート

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