Water → HCID 68138675, 화합물

HRID 268241

반응식

HRID 268241 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 68138675HCID 68138675, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9aee42b105fd42508b68c12497ef38d1
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947434

연결된 노트

불러오는 중…