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Ethyl Acetate → HCID 68313136、化合物

HRID 1530444
ノート
印刷プレビュー

反応式

HRID 1530444 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C([O:9][C:10](=O)[CH:11]([O:20][C:21]1[CH:43]=[CH:42][C:24]2[C:25]3[N:29]([CH2:30][CH2:31][O:32][C:23]=2[CH:22]=1)[CH:28]=[C:27]([C:33]1[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=1)[N:26]=3)[CH2:12][CH:13]([CH3:19])[C:14](OCC)=[O:15])C.CCOC(C)=O.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1COCC1>[CH:39]([N:34]1[C:33]([C:27]2[N:26]=[C:25]3[N:29]([CH2:30][CH2:31][O:32][C:23]4[CH:22]=[C:21]([O:20][CH:11]([CH2:12][CH:13]([CH3:19])[CH2:14][OH:15])[CH2:10][OH:9])[CH:43]=[CH:42][C:24]=43)[CH:28]=2)=[N:37][C:36]([CH3:38])=[N:35]1)([CH3:41])[CH3:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 9357Potassium Sodium TartrateHCID 21226445Aluminium lithium hydrideHCID 68313011HCID 68313011、化合物

生成物 1

HCID 68313136HCID 68313136、化合物収率 55.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒
2 回

実験手順

To a suspension of LiAlH4 (85 mg, 2.23 mmol) in THF (1 mL) at 0° C. was added a solution of 2-[2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]-4-methylpentanedioic acid diethyl ester (391 mg, 0.744 mmol) in THF (20 mL) and stirring at RT was continued for 2.5 h. To the reaction mixture was added EtOAc (2 mL) and stirring was continued for 30 min. An aqueous solution (10%) of Rochelle's salt was then added and the mixture was stirred for 5 min. Organic solvents were removed under reduced pressure and the resulting aqueous phase was extracted with EtOAc (×2). The combined organic phases were washed with water, followed by brine, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 3-18% MeOH in DCM) affording 2-[2-(2-Isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]-4-methylpentane-1,5-diol as a colorless gum (181 mg, 55%). LCMS: RT 2.49 min [M+H]+ 442.3

後処理

  1. stirringstirring
  2. waitwas continued for 30 min
  3. stirringthe mixture was stirred for 5 min
  4. customOrganic solvents were removed under reduced pressure
  5. extractionthe resulting aqueous phase was extracted with EtOAc (×2)
  6. washThe combined organic phases were washed with water
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 3-18% MeOH in DCM)

出典と根拠

ORDレコード
ord-c3af069f89194c288b84f93fab65bcc0
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

反応ノート

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