Sulfuric Acid → HCID 20502722、化合物

HRID 851165ノート

反応式

HRID 851165 の反応式
[C:1]([C:3]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][CH2:5][CH:4]=1)#N.[H-].C([Al+]CC(C)C)C(C)C.[OH:23]S(O)(=O)=O>C1C=CC=CC=1.C1(C)C=CC=CC=1>[CH:1]([C:3]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][CH2:5][CH:4]=1)=[O:23]

参加物

6

反応物 3

HCID 1118Sulfuric AcidHCID 132277052H-1-Benzothiopyran-4-carbonitrileHCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 20502722HCID 20502722、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 1140Toluene溶媒

実験手順

0.5 g of 4-cyano-2H-1-benzothiopyrane in 2 ml of benzene are reacted with 2 ml of a 20% solution of diisobutylaluminium hydride in toluene and the mixture stirred for 4 hours at room temperature. The resulting mixture is poured onto 20% H2SO4 and the organic phase separated, washed with saturated aqueous NaCl and dried over MgSO4. After concentration by evaporation the product is purified by chromatography over kieselgel (eluant hexane/ethyl acetate).

後処理

  1. customthe organic phase separated
  2. washwashed with saturated aqueous NaCl
  3. dry with materialdried over MgSO4
  4. concentrationAfter concentration
  5. customby evaporation the product
  6. customis purified by chromatography over kieselgel (eluant hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-2e338e6c31cf4deeba09d532a7e12bd2
出典データセット
uspto-grants-1983_05
特許番号
US04382951

反応ノート

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