Potassium Acetate → HCID 22397176, 화합물

HRID 411226노트

반응식

HRID 411226 반응식
[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[C:10](Cl)[N:11]=[C:12]([CH2:17][N:18]3[CH2:23][CH2:22][O:21][CH2:20][CH2:19]3)[CH:13]=2)[N:8]([CH3:25])[CH:7]=1)=[O:5])[CH3:2].C([O-])(=O)C.[K+]>C(O)(C)C.[Pd]>[CH2:1]([O:3][C:4]([C:6]1[C:15](=[O:16])[C:14]2[C:9](=[CH:10][N:11]=[C:12]([CH2:17][N:18]3[CH2:19][CH2:20][O:21][CH2:22][CH2:23]3)[CH:13]=2)[N:8]([CH3:25])[CH:7]=1)=[O:5])[CH3:2]

참가 물질

5

반응물 2

HCID 517044Potassium AcetateHCID 22397142HCID 22397142, 화합물

생성물 1

HCID 22397176HCID 22397176, 화합물수율 711.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 3776Isopropanol용매

실험 절차

A mixture of ethyl-8-chloro-1-methyl-6-(4-morpholinylmethyl)-4-oxo-1,4-dihydro-[1,7]naphthyridine-3-carboxylate (Preparation 45, 0.090 g), potassium acetate (0.015 g) and 10% Pd/C (20 mg) in isopropyl alcohol is hydrogenated (balloon) for 18 hours. The mixture is filtered through celite and the filter cake washed with MeOH. The solvent is evaporated and the crude solid chromatographed with CH2Cl2\CH3OH\TEA (90\9\1) to obtain 0.58 g (70%) of the title compound as an off-white solid. Physical characteristics: MS (ESI+) m/z 332 (M+H).

후처리

  1. customfor 18 hours
  2. filtrationThe mixture is filtered through celite
  3. washthe filter cake washed with MeOH
  4. customThe solvent is evaporated
  5. customthe crude solid chromatographed with CH2Cl2\CH3OH\TEA (90\9\1)

출처 및 근거

ORD 기록
ord-21f3a8e2dd974b25bf6c71308ac5e06d
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559145B2

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