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Sodium Acetate Trihydrate → HCID 59540666, 화합물

HRID 1677515
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HRID 1677515 반응식
[CH3:1][C:2]([CH3:37])([CH2:34][CH:35]=[CH2:36])[C:3]([C:5]1[C:13]2[C:8](=[N:9][CH:10]=[C:11]([C:14]3[CH:19]=[C:18]([O:20][CH3:21])[C:17]([O:22][CH3:23])=[C:16]([O:24][CH3:25])[CH:15]=3)[N:12]=2)[N:7](COCC[Si](C)(C)C)[CH:6]=1)=[O:4].O.O.O.C([O-])(=O)C.[Na+]>ClCCl.FC(F)(F)C(O)=O>[CH3:1][C:2]([CH3:37])([CH2:34][CH:35]=[CH2:36])[C:3]([C:5]1[C:13]2[C:8](=[N:9][CH:10]=[C:11]([C:14]3[CH:19]=[C:18]([O:20][CH3:21])[C:17]([O:22][CH3:23])=[C:16]([O:24][CH3:25])[CH:15]=3)[N:12]=2)[NH:7][CH:6]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 23665404Sodium Acetate TrihydrateHCID 595408992,2-dimethyl-1-[2-(3,4,5-trimethoxy-phenyl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-pent-4-en-1-one

생성물 1

HCID 59540666HCID 59540666, 화합물수율 50.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid
용매

실험 절차

A solution of 2,2-dimethyl-1-[2-(3,4,5-trimethoxy-phenyl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-pent-4-en-1-one (0.127 g, 0.242 mmol) in 4 mL of dichloromethane and 1 mL of trifluoroacetic acid was stirred for 3 h, then concentrated. The residue was taken up in 2 mL of ethanol (not all dissolves) and treated with sodium acetate trihydrate (0.329 g, 2.42 mmol). The mixture was stirred for 4 d, then concentrated to a residue. Column chromatography (0→5% MeOH/CH2Cl2) afforded 0.048 g (50%) of 2,2-dimethyl-1-[2-(3,4,5-trimethoxy-phenyl)-5H-pyrrolo[2,3-b]pyrazin-7-yl]-pent-4-en-1-one as a white solid.

후처리

  1. concentrationconcentrated
  2. dissolutionall dissolves) and
  3. concentrationconcentrated to a residue

출처 및 근거

ORD 기록
ord-0ba71146db1b4248ad1d377e30e74b37
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008298B2

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