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Water → HCID 18448155, 화합물

HRID 1269359
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HRID 1269359 반응식
[C:1](=[O:34])([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][O:30][N+:31]([O-:33])=[O:32])[O:2][CH2:3]/[C:4](/[C:14]1[CH:19]=[CH:18][C:17]([S:20]([CH3:23])(=[O:22])=[O:21])=[CH:16][CH:15]=1)=[C:5](/[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)\[CH2:6][OH:7].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=[O:37].O.OP(O)(O)=O.[O-]Cl=O.[Na+].CC(=CC)C>ClCCl.CCOC(C)=O>[CH3:23][S:20]([C:17]1[CH:18]=[CH:19][C:14](/[C:4](/[CH2:3][O:2][C:1]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][O:30][N+:31]([O-:33])=[O:32])=[O:34])=[C:5](\[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)/[C:6]([OH:37])=[O:7])=[CH:15][CH:16]=1)(=[O:21])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 6

HCID 962WaterHCID 1004Phosphoric AcidHCID 105532-Methyl-2-buteneHCID 159087TriacetoxyperiodinaneHCID 23668197Sodium ChloriteHCID 58841190HCID 58841190, 화합물

생성물 1

HCID 18448155
HCID 18448155, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of (2Z)-4-hydroxy-2-[4-(methylsulfonyl)phenyl]-3-phenylbut-2-enyl 5-(nitrooxy)pentyl carbonate (1 eq, 0.2M) in dichloromethane was treated with Dess-Martin reagent (1.3 eq) for 1 h at rt. The reaction was quenched by 10 eq of water and stirred at rt for 1 h, filtered on a silica gel pad eluted with 60% EtOAc/hexanes and evaporated. The residue was dissolved in a 3:1 solvent mixture of tBuOH/CH2Cl2, and treated with 1 M H3PO4 (4 eq) and 1 M NaClO2 (2 eq) in the presence of an excess of 2-methyl-2-butene. The resulting mixture was stirred at rt for 30 min, diluted with EtOAc and the organic layer was separated, washed with brine, dried (Na2SO4), and evaporated to afford the crude acid used as such for next step.

후처리

  1. filtrationfiltered on a silica gel pad
  2. washeluted with 60% EtOAc/hexanes
  3. customevaporated
  4. dissolutionThe residue was dissolved in a 3:1 solvent mixture of tBuOH/CH2Cl2
  5. stirringThe resulting mixture was stirred at rt for 30 min
  6. customthe organic layer was separated
  7. washwashed with brine
  8. dry with materialdried (Na2SO4)
  9. customevaporated

출처 및 근거

ORD 기록
ord-3bfb3160616c4937b7f2ca1d0899226d
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07199154B2

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