Lithium hydroxide, monohydrate → 17-[2-(3-Isopropylpyrazol-1-yl)-7-methoxy-8-methylquinazolin-4-yloxy]-13-methyl-2,14-dioxo-3,13-diazatricyclo[13.3.0.04,6]octadec-7-ene-4-carboxylic acid

HRID 1443496ノート

反応式

HRID 1443496 の反応式
O.[OH-].[Li+].C([O:6][C:7]([C:9]12[CH2:26][CH:25]1[CH:24]=[CH:23][CH2:22][CH2:21][CH2:20][CH2:19][N:18]([CH3:27])[C:17](=[O:28])[CH:16]1[CH:12]([CH2:13][CH:14]([O:29][C:30]3[C:39]4[C:34](=[C:35]([CH3:42])[C:36]([O:40][CH3:41])=[CH:37][CH:38]=4)[N:33]=[C:32]([N:43]4[CH:47]=[CH:46][C:45]([CH:48]([CH3:50])[CH3:49])=[N:44]4)[N:31]=3)[CH2:15]1)[C:11](=[O:51])[NH:10]2)=[O:8])C>O.C1COCC1>[CH:48]([C:45]1[CH:46]=[CH:47][N:43]([C:32]2[N:31]=[C:30]([O:29][CH:14]3[CH2:13][CH:12]4[CH:16]([C:17](=[O:28])[N:18]([CH3:27])[CH2:19][CH2:20][CH2:21][CH2:22][CH:23]=[CH:24][CH:25]5[C:9]([C:7]([OH:8])=[O:6])([NH:10][C:11]4=[O:51])[CH2:26]5)[CH2:15]3)[C:39]3[C:34](=[C:35]([CH3:42])[C:36]([O:40][CH3:41])=[CH:37][CH:38]=3)[N:33]=2)[N:44]=1)([CH3:50])[CH3:49]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 68688284HCID 68688284、化合物

生成物 1

HCID 6868954017-[2-(3-Isopropylpyrazol-1-yl)-7-methoxy-8-methylquinazolin-4-yloxy]-13-methyl-2,14-dioxo-3,13-diazatricyclo[13.3.0.04,6]octadec-7-ene-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of lithium hydroxide hydrate (796 mg, 18.6 mmol) in water (10 mL) was added to a stirred solution of the ester (145) (346 mg, 0.526 mmol) in THF (30 mL). After 5 days at room temperature, the reaction mixture was concentrated under vacuum. The pH was adjusted to 4 with 1N HCl and the resulting solution was successively extracted with AcOEt, washed with brine, dried (Na2SO4) and evaporated.

後処理

  1. concentrationthe reaction mixture was concentrated under vacuum
  2. extractionthe resulting solution was successively extracted with AcOEt
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated

出典と根拠

ORDレコード
ord-456e7c9b35144961b7548638a99cd33f
出典データセット
uspto-grants-2010_02
特許番号
US07659245B2

反応ノート

読み込み中…