Water → HCID 68138675、化合物

HRID 268241

反応式

HRID 268241 の反応式
[N+:1]([C:4]1[CH:12]=[CH:11][C:7]2[N:8]=[CH:9][NH:10][C:6]=2[CH:5]=1)([O-])=O.O.[C:14]([O:20][CH2:21][CH3:22])(=[O:19])[CH2:15][C:16]([CH3:18])=O.S([O-])([O-])(=O)=O.[Ca+2]>C(O)C.[Pd].CC(O)=O>[N:8]1[C:7]2[CH:11]=[CH:12][C:4]([NH:1]/[C:16](/[CH3:18])=[CH:15]\[C:14]([O:20][CH2:21][CH3:22])=[O:19])=[CH:5][C:6]=2[NH:10][CH:9]=1

参加物

8

反応物 4

HCID 962WaterHCID 71955-NitrobenzimidazoleHCID 8868Ethyl AcetoacetateHCID 24497Calcium Sulfate

生成物 1

HCID 68138675HCID 68138675、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

実験手順

An 82 g. (0.5 mole) sample of 5-nitrobenzimidazole in 900 ml of ethanol was reduced over 4 g. of 5% Pd/C catalyst containing 50% H2O. After a pressure drop of 108 lb. (calcd. 106 lb.), the reduction stopped. After filtration of the catalyst, 65 g. (0.5 mole) of ethyl acetoacetate, 20 g. of anhydrous calcium sulfate, and 0.5 ml of HOAc was added. After filtration of the anhydrous calcium sulfate the solution was concentrated in vacuo till till a solid remained. The product was filtered and washed with fresh ethanol and air-dried. The yield was 84 g. (69%), m.p. 160°-162°C.

後処理

  1. filtrationAfter filtration of the catalyst, 65 g
  2. filtrationAfter filtration of the anhydrous calcium sulfate the solution
  3. concentrationwas concentrated in vacuo till till a solid
  4. filtrationThe product was filtered
  5. washwashed with fresh ethanol
  6. customair-dried

出典と根拠

ORDレコード
ord-9aee42b105fd42508b68c12497ef38d1
出典データセット
uspto-grants-1976_03
特許番号
US03947434

関連ノート

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