Sodium Hydroxide → HCID 67154626, 화합물

HRID 83086노트

반응식

HRID 83086 반응식
[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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 21226129Dichloromethane methanolHCID 68338070HCID 68338070, 화합물

생성물 1

HCID 67154626HCID 67154626, 화합물수율 48%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0eb5533118bf45e9bca79a5c6d570320
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846711B2

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