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Methanol → HCID 21201815, 화합물

HRID 1979452
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HRID 1979452 반응식
[C:1]1([C:6]([CH2:8][N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[N:13]([CH:20]3[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]3)[CH2:12][CH:11]([NH:26][C:27]([NH:29][C:30]3[CH:35]=[CH:34][C:33](C(OCC)=O)=[CH:32][CH:31]=3)=[O:28])[C:10]2=[O:41])=O)[S:5][CH:4]=[CH:3][CH:2]=1.[OH2:42].[OH-:43].[Li+].[CH3:45][OH:46]>O1CCCC1>[C:1]1([C:6]([CH2:8][N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[N:13]([CH:20]3[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]3)[CH2:12][CH:11]([NH:26][C:27](=[O:28])[NH:29][C:30]3[CH:35]=[C:34]([CH:33]=[CH:32][CH:31]=3)[C:45]([OH:46])=[O:43])[C:10]2=[O:41])=[O:42])[S:5][CH:4]=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 21201786HCID 21201786, 화합물

생성물 1

HCID 21201815HCID 21201815, 화합물수율 92.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
45 °C

실험 절차

1-[1-(2-Thenoylmethyl)-2-oxo-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(4-ethoxycarbonylphenyl)urea (0.70 g) was dissolved in tetrahydrofuran (19 ml), aqueous lithium hydroxide monohydrate (0.26 g) solution (15 ml) and methanol (7 ml) were added, the mixture was stirred at 40-50° C. for one hours. The reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid and chloroform were added to the residue, and extracted. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, a mixed solvent of methylene chloride and ether (1:1) was added to powder so precipitated, and collected by filtration,to thereby obtain 0.61 g of the title compound (Yield: 92.4%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, 1N hydrochloric acid and chloroform
  2. additionwere added to the residue
  3. extractionextracted
  4. washThe organic layer was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. additiona mixed solvent of methylene chloride and ether (1:1) was added to powder
  8. customso precipitated
  9. filtrationcollected by filtration,to

출처 및 근거

ORD 기록
ord-5bbbab4aa233464fbc7a9f023ebc9870
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06239131B1

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