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Sodium borohydride → HCID 15522057, 화합물

HRID 1859028
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HRID 1859028 반응식
[N+:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:13]=1[O:12][CH2:11][CH2:10][C:9]2=O)([O-:3])=[O:2].[BH4-].[Na+]>C(O)C>[N+:1]([C:4]1[CH:5]=[CH:6][CH:7]=[C:8]2[C:13]=1[O:12][CH2:11][CH:10]=[CH:9]2)([O-:3])=[O:2]
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 186797008-Nitro-2,3-dihydro-4H-1-benzopyran-4-one

생성물 1

HCID 15522057HCID 15522057, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 20 g of 8-nitro-4-chromanone and 3.9 g of sodium borohydride in 200 ml of ethanol is heated at reflux for 45 minutes and then evaporated to dryness. The residue is taken up in 200 ml of water and extracted three times with 250 ml of dichloromethane each time. The combined organic phases are dried over magnesium sulphate, filtered and then concentrated under reduced pressure. The liquid residue is taken up in 300 ml of toluene; 0.5 g of para-toluenesulphonic acid is then added and heating at reflux is carried out until the full amount of water expected has been recovered. After cooling, washing with a 5% sodium carbonate solution and then with water, and concentrating under reduced pressure, a liquid residue corresponding to the expected product is isolated.

후처리

  1. temperatureat reflux for 45 minutes
  2. customevaporated to dryness
  3. extractionextracted three times with 250 ml of dichloromethane each time
  4. dry with materialThe combined organic phases are dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. addition0.5 g of para-toluenesulphonic acid is then added
  8. temperatureheating
  9. temperatureat reflux
  10. customexpected has been recovered
  11. temperatureAfter cooling
  12. washwashing with a 5% sodium carbonate solution
  13. concentrationwith water, and concentrating under reduced pressure

출처 및 근거

ORD 기록
ord-a571f1ce06fd42c4979d73a586f5ec89
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06153625

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