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Lithium Hydroxide → L-796449

HRID 342765
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HRID 342765 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:31][C:32]([O:34]C)=[O:33])[CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:27]=[CH:26][C:16]2[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:18][O:19][C:15]=2[C:14]=1[CH2:28][CH2:29][CH3:30].[OH-].[Li+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:31][C:32]([OH:34])=[O:33])[CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:27]=[CH:26][C:16]2[C:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)=[CH:18][O:19][C:15]=2[C:14]=1[CH2:28][CH2:29][CH3:30]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 15840674HCID 15840674, 화합물

생성물 1

HCID 9891946L-796449

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of methyl 3-chloro-4-(3-(3-phenyl-7-propylbenzofuran-6-yloxy)propylthio)-phenylacetate (3.72 g, 7.31 mmol) prepared in last step and aqueous lithium hydroxide(1.0M; 14.62 ml; 14.62 mmol) in methanol (25 ml) was refluxed for 1 hr. The mixture was partitioned between isopropyl acetate and pH4 buffer. The organic was dried over sodium sulfate. The solvent was removed under reduced pressure, and the residue was purified by chromatography (silica gel, 50% methylene chloride in hexane) to afford the title compound. M.P: 143° C. ESI-MS: m/e-495(M+1)

후처리

  1. temperaturewas refluxed for 1 hr
  2. customThe mixture was partitioned between isopropyl acetate and pH4 buffer
  3. dry with materialThe organic was dried over sodium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by chromatography (silica gel, 50% methylene chloride in hexane)

출처 및 근거

ORD 기록
ord-702b7fddd92c4e96aef65430aa960667
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859051

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