Sodium Hydroxide → HCID 67154626、化合物

HRID 83086ノート

反応式

HRID 83086 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][C:5]2([CH2:16][C:15]3[C:10](=[N:11][CH:12]=[C:13](/[CH:17]=[CH:18]/[C:19]([O:21]CC)=[O:20])[CH:14]=3)[NH:9][C:8]2=[O:24])[CH2:4][CH2:3]1.[OH-].[Na+].C(Cl)[Cl:28].CO>C(Cl)Cl.CCO>[ClH:28].[CH3:1][N:2]1[CH2:3][CH2:4][C:5]2([CH2:16][C:15]3[C:10](=[N:11][CH:12]=[C:13](/[CH:17]=[CH:18]/[C:19]([OH:21])=[O:20])[CH:14]=3)[NH:9][C:8]2=[O:24])[CH2:6][CH2:7]1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 68338070HCID 68338070、化合物

生成物 1

HCID 67154626HCID 67154626、化合物収率 48%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of (E)-ethyl 3-(1′-methyl-2-oxo-2,4-dihydro-1H-spiro[[1,8]naphthyridine-3,4′-piperidine]-6-yl)acrylate (95 mg, 0.288 mmol) in DCM (2 mL) and EtOH (2 mL) was added 1N aqueous sodium hydroxide (1 mL, 1.000 mmol) and the reaction was stirred at rt overnight, after which TLC (DCM/MeOH, 9:1) showed full conversion. Next, the mixture was concentrated and the residue acidified with 1N HCl (5 mL) and stirred for 1 h. The resulting white solids were isolated by filtration, washed with H2O and Et2O and dried on the filter. The product (47 mg, 48%) was obtained as an off-white solid.

後処理

  1. concentrationNext, the mixture was concentrated
  2. stirringstirred for 1 h
  3. customThe resulting white solids were isolated by filtration
  4. washwashed with H2O and Et2O
  5. customdried on the filter

出典と根拠

ORDレコード
ord-0eb5533118bf45e9bca79a5c6d570320
出典データセット
uspto-grants-2014_09
特許番号
US08846711B2

反応ノート

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