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Methanol → 5-(13-Cyclohexyl-10-((isopropylsulfonyl)carbamoyl)-3-methoxy-7h-indolo[2,1-a][2]benzazepin-6-yl)-1-ethyl-1h-pyrazole-4-carboxylic acid

HRID 1097807
ノート
印刷プレビュー

反応式

HRID 1097807 の反応式
[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:39](=[O:47])[NH:40][S:41]([CH:44]([CH3:46])[CH3:45])(=[O:43])=[O:42])=[CH:12][C:13]=3[N:14]3[CH2:20][C:19]([C:21]4[N:25]([CH2:26][CH3:27])[N:24]=[CH:23][C:22]=4[C:28]([O:30]CC)=[O:29])=[CH:18][C:17]4[CH:33]=[C:34]([O:37][CH3:38])[CH:35]=[CH:36][C:16]=4[C:15]=23)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CO.[OH-].[Na+]>C1COCC1>[CH:1]1([C:7]2[C:8]3[CH:9]=[CH:10][C:11]([C:39](=[O:47])[NH:40][S:41]([CH:44]([CH3:46])[CH3:45])(=[O:42])=[O:43])=[CH:12][C:13]=3[N:14]3[CH2:20][C:19]([C:21]4[N:25]([CH2:26][CH3:27])[N:24]=[CH:23][C:22]=4[C:28]([OH:30])=[O:29])=[CH:18][C:17]4[CH:33]=[C:34]([O:37][CH3:38])[CH:35]=[CH:36][C:16]=4[C:15]=23)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1
参加物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 14798Sodium HydroxideHCID 57948826Ethyl 5-(13-cyclohexyl-10-((isopropylsulfonyl)carbamoyl)-3-methoxy-7h-indolo[2,1-a][2]benzazepin-6-yl)-1-ethyl-1h-pyrazole-4-carboxylate

生成物 1

HCID 468931605-(13-Cyclohexyl-10-((isopropylsulfonyl)carbamoyl)-3-methoxy-7h-indolo[2,1-a][2]benzazepin-6-yl)-1-ethyl-1h-pyrazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Ethyl 5-(13-cyclohexyl-10-((isopropylsulfonyl)carbamoyl)-3-methoxy-7H-indolo[2,1-a][2]benzazepin-6-yl)-1-ethyl-1H-pyrazole-4-carboxylate was dissolved in THF (14 mL) and methanol (14 mL) then sodium hydroxide (15 mL, 15.00 mmol) (1.0N aqueous) was added to the reaction. The reaction was placed under a nitrogen atmosphere and stirred at room temperature for 16.5 hrs. The reaction was concentrated in vacuo using a rotary evaporator (bath temp equal to less than 26 C) then partitioned between ethyl acetate and 1.0N aqueous hydrochloric acid. The aqueous layer was extracted with ethyl acetate and the organic extracts combined, washed with brine and dried over magnesium sulfate. The organic solution was filtered and solvents removed in vacuo to give amorphous amber-orange solid (902 mg) after drying at room temperature in vacuo.

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. customa rotary evaporator (bath temp equal to less than 26 C)
  3. customthen partitioned between ethyl acetate and 1.0N aqueous hydrochloric acid
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationThe organic solution was filtered
  8. customsolvents removed in vacuo

出典と根拠

ORDレコード
ord-2c11d508101f436680bfb71a3d4e5cd8
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143243B2

反応ノート

読み込み中…

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