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Sodium Hydroxide → HCID 90408458、化合物

HRID 871103
ノート
印刷プレビュー

反応式

HRID 871103 の反応式
[O:1]1[CH2:6][CH2:5][CH:4]([CH2:7][N:8]2[C:12]3[CH:13]=[C:14]([C:17]4[CH:22]=[CH:21][N:20]=[C:19]5[N:23](S(C6C=CC(C)=CC=6)(=O)=O)[C:24]([C:26]6[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:28][CH:27]=6)=[CH:25][C:18]=45)[CH:15]=[CH:16][C:11]=3[N:10]=[N:9]2)[CH2:3][CH2:2]1.[OH-].[Na+]>O1CCOCC1>[O:1]1[CH2:2][CH2:3][CH:4]([CH2:7][N:8]2[C:12]3[CH:13]=[C:14]([C:17]4[CH:22]=[CH:21][N:20]=[C:19]5[NH:23][C:24]([C:26]6[CH2:31][CH2:30][N:29]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:28][CH:27]=6)=[CH:25][C:18]=45)[CH:15]=[CH:16][C:11]=3[N:10]=[N:9]2)[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

4

反応物 2

HCID 14798Sodium HydroxideHCID 90409594tert-butyl 4-(4-(1-((tetrahydro-2H-pyran-4-yl)methyl)-1H-benzo[d][1,2,3]triazol-6-yl)-1-tosyl-1H-pyrrolo[2,3-b]pyridin-2-yl)-5,6-dihydropyridine-1(2H)-carboxylate

生成物 1

HCID 90408458HCID 90408458、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of Example 36E (0.530 g, 0.792 mmol) and 5M aqueous sodium hydroxide (0.555 mL, 2.77 mmol) in dioxane (8 mL) was heated at 90° C. for 8 hours. The solvent was evaporated and the residue was treated with ethyl acetate and washed with aqueous NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated until most of solvent was evaporated. The resulting precipitate was filtered, washed with ethyl acetate/ether, and vacuum oven-dried to give the title compound. The filtrate was concentrated and purified on a 4 g column using the ISCO Companion flash system eluting with ethyl acetate to give additional title compound.

後処理

  1. customThe solvent was evaporated
  2. additionthe residue was treated with ethyl acetate
  3. washwashed with aqueous NaHCO3
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated until most of solvent
  7. customwas evaporated
  8. filtrationThe resulting precipitate was filtered
  9. washwashed with ethyl acetate/ether, and vacuum
  10. customoven-dried

出典と根拠

ORDレコード
ord-b622bf51268944fc803d88513c92e216
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969375B2

反応ノート

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