Sodium Hydroxide → HCID 68580202、化合物

HRID 644377ノート

反応式

HRID 644377 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:9][CH:10]([NH:16][C:17]([N:19]2[CH2:24][CH2:23][CH:22]([N:25]3[CH2:34][C:33]4[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=4)[NH:27][C:26]3=[O:35])[CH2:21][CH2:20]2)=[O:18])[C:11]([O:13]CC)=[O:12])[CH:5]=[CH:6][C:7]=1[CH3:8].[OH-].[Na+]>CO>[CH3:1][C:2]1[CH:3]=[C:4]([CH2:9][CH:10]([NH:16][C:17]([N:19]2[CH2:24][CH2:23][CH:22]([N:25]3[CH2:34][C:33]4[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=4)[NH:27][C:26]3=[O:35])[CH2:21][CH2:20]2)=[O:18])[C:11]([OH:13])=[O:12])[CH:5]=[CH:6][C:7]=1[CH3:8]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 68579013ethyl 3-(3,4-dimethyl-phenyl)-2-{[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidine-1-carbonyl]-amino}-propionate

生成物 1

HCID 68580202HCID 68580202、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

17.5 g (36.6 mmol) ethyl 3-(3,4-dimethyl-phenyl)-2-{[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidine-1-carbonyl]-amino}-propionate dissolved in 100 mL MeOH was combined with 200 mL 1 M NaOH and stirred overnight at RT. The reaction mixture was filtered, the filtrate washed three times with tert-butylmethylether and combined with 200 mL 1 M HCl. The aqueous phase was extracted three times with EtOAc, the combined organic phases were dried, filtered and evaporated down under reduced pressure. The residue was triturated with diisopropylether, suction filtered, stirred with diethyl ether and dried at 50° C. in the circulating air dryer.

後処理

  1. filtrationThe reaction mixture was filtered
  2. washthe filtrate washed three times with tert-butylmethylether
  3. extractionThe aqueous phase was extracted three times with EtOAc
  4. customthe combined organic phases were dried
  5. filtrationfiltered
  6. customevaporated down under reduced pressure
  7. customThe residue was triturated with diisopropylether, suction
  8. filtrationfiltered
  9. stirringstirred with diethyl ether
  10. customdried at 50° C. in the circulating air dryer

出典と根拠

ORDレコード
ord-1c0bd74828c24965ad0d5389e01cebec
出典データセット
uspto-grants-2010_04
特許番号
US07700589B2

反応ノート

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