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Methanol → HCID 21201815、化合物

HRID 1979452
ノート
印刷プレビュー

反応式

HRID 1979452 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 168937Lithium hydroxide, monohydrateHCID 21201786HCID 21201786、化合物

生成物 1

HCID 21201815HCID 21201815、化合物収率 92.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-5bbbab4aa233464fbc7a9f023ebc9870
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06239131B1

反応ノート

読み込み中…

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