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Citric Acid → HCID 17805852, 화합물

HRID 365698
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HRID 365698 반응식
C([O:4][CH2:5][C:6]1[CH:11]=[C:10]([CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[CH:9]=[C:8]([CH2:23][O:24]C(=O)C)[N:7]=1)(=O)C.C(OCC1C=C(CCC2C=CC([N+]([O-])=O)=CC=2)C=C(C)N=1)(=O)C.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C(O)C>[OH:24][CH2:23][C:8]1[CH:9]=[C:10]([CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=2)[CH:11]=[C:6]([CH2:5][OH:4])[N:7]=1
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참가 물질

5

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HCID 311Citric AcidHCID 232929272-Pyridinemethanol, 6-methyl-4-[2-(4-nitrophenyl)ethyl]-, 2-acetateHCID 57103833HCID 57103833, 화합물

생성물 1

HCID 17805852HCID 17805852, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Diacetate (7) (12.0 g, 34.1 mmol), was dissolved in 50 ml of ethanol. To this solution stirred at RT, sodium hydroxide 5 H, 20 ml was added at once. After 10 min, when the TLC test for the substrate was negative, the mixture was neutralized with citric acid, and partitioned between sat. sodium hydrogen carbonate and ethanol/chloroform 1:1. The extraction was repeated three times using 100 ml of organic solvent for each extraction. The combined extracts were evaporated and the residual mixture was flash chromatographed using finally 8% ethanol/ chloroform as a solvent. The appropriate pure fractions were collected and evaporated.

후처리

  1. custompartitioned between sat. sodium hydrogen carbonate and ethanol/chloroform 1:1
  2. extractionThe extraction
  3. extractionfor each extraction
  4. customThe combined extracts were evaporated
  5. customchromatographed
  6. customThe appropriate pure fractions were collected
  7. customevaporated

출처 및 근거

ORD 기록
ord-2b5d97dedaba41d6b61869be5f96df69
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06127529

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