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Ethanol → HCID 178513659, 화합물

HRID 1625210
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HRID 1625210 반응식
[OH:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:9]2[CH:16]=[C:15]([N:17]3[C:21]4=[N:22][CH:23]=[CH:24][C:25]([C:26]5[CH:27]=[N:28][C:29]6[C:34]([CH:35]=5)=[CH:33][CH:32]=[CH:31][CH:30]=6)=[C:20]4[C:19]([C:36]([F:39])([F:38])[F:37])=[N:18]3)[CH:14]=[CH:13][C:10]=2[C:11]#[N:12])[CH2:4][CH2:3]1.C([OH:42])C.[OH-].[Na+].OO>CS(C)=O.O.C(OCC)(=O)C>[OH:1][C@H:2]1[CH2:3][CH2:4][C@H:5]([NH:8][C:9]2[CH:16]=[C:15]([N:17]3[C:21]4=[N:22][CH:23]=[CH:24][C:25]([C:26]5[CH:27]=[N:28][C:29]6[C:34]([CH:35]=5)=[CH:33][CH:32]=[CH:31][CH:30]=6)=[C:20]4[C:19]([C:36]([F:39])([F:38])[F:37])=[N:18]3)[CH:14]=[CH:13][C:10]=2[C:11]([NH2:12])=[O:42])[CH2:6][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 702EthanolHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 178510018HCID 178510018, 화합물

생성물 1

HCID 178513659HCID 178513659, 화합물수율 65%

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매2회
HCID 962Water용매2회
HCID 8857Ethyl Acetate용매

실험 절차

Compound (1f) (0.450 g) was dissolved in dimethyl sulfoxide (hereinafter referred to as DMSO, 2 mL) and ethanol (4 mL). An aqueous sodium hydroxide solution (4 M, 0.851 mL) and a 30% hydrogen peroxide solution (0.193 mL) were added to the resulting solution in this order at room temperature, followed by stirring for 30 min. Water was added to the reaction solution, the reaction solution was distributed between ethyl acetate and water, and the organic layer was washed with saturated saline. The organic layer after the washing was dried over anhydrous sodium sulfate, and then the solvent was distilled away. The residue was purified by neutral silica gel column chromatography (chloroform/methanol) to obtain compound (1) (0.300 g, 65%) as a white solid.

후처리

  1. washthe organic layer was washed with saturated saline
  2. dry with materialThe organic layer after the washing was dried over anhydrous sodium sulfate
  3. distillationthe solvent was distilled away
  4. customThe residue was purified by neutral silica gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-eddd1e6bd28c454b8247f5c4d856e6b2
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08779142B2

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