Acetic Acid → HCID 18355461, 화합물

HRID 429335노트

반응식

HRID 429335 반응식
[CH2:1]([O:3][C:4]([CH2:6][C:7]([C:9]1[O:10][C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[CH:13]=1)=O)=[O:5])[CH3:2].[BH4-].[Na+].C(O)(=O)C>C(O)C.O.[Pd]>[O:10]1[C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[CH:13]=[C:9]1[CH2:7][CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5]

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 4311764Sodium borohydride2회HCID 12777066Ethyl 3-(1-benzofuran-2-yl)-3-oxopropanoate

생성물 1

HCID 18355461HCID 18355461, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

232 g of compound 3 are dissolved in 500 ml of ethanol. Cool in ice-bath and add 100 g of sodium borohydride in 500 ml of water. Stir for 2 hours. Add acetic acid until the sodium borohydride has been neutralized. Cool the solution in ice-bath under an atmosphere of nitrogen and add 10 g of 10% Pd/C catalyst. Stir under a hydrogen atmosphere at 15PSI until the reaction is complete, as judged by TLC. Filter through celite and evaporate organic solvents. Extract with ethyl acetate. Dry over sodium sulfate. Filter. Evaporate solvent.

후처리

  1. temperatureCool in ice-bath
  2. temperatureCool the solution in ice-bath under an atmosphere of nitrogen
  3. stirringStir under a hydrogen atmosphere at 15PSI until the reaction
  4. filtrationFilter through celite
  5. customevaporate organic solvents
  6. extractionExtract with ethyl acetate
  7. dry with materialDry over sodium sulfate
  8. filtrationFilter

출처 및 근거

ORD 기록
ord-5ef3d64006d046358df24148c5752c4e
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316487B1

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