Water → HCID 68874499, 화합물

HRID 2366636노트

반응식

HRID 2366636 반응식
[N+:1]([C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[NH:14][CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=[CH:9][CH:8]=2)([O-])=O.S(S([O-])=O)([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+].O>CC[N+]1C=CC(C2C=C[N+](CC)=CC=2)=CC=1.[Br-].[Br-].ClCCl>[NH2:1][C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[NH:14][CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=[CH:9][CH:8]=2

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 24489Sodium Dithionite2회HCID 68873567HCID 68873567, 화합물

생성물 1

HCID 68874499HCID 68874499, 화합물

시약·촉매·용매 2

HCID 114742621,1'-Diethyl-4,4'-bipyridinium dibromide촉매HCID 6344Dichloromethane용매

실험 절차

Ethyl N-(3-nitroquinolin-4-yl)-β-alaninate (62.0 g, 214 mmol, prepared as described in Part A of Example 15) was treated with sodium hydrosulfite (130.6 g, 750.1 mmol), potassium carbonate (117 g, 847 mmol), and ethyl viologen dibromide (0.802 g, 2.14 mmol) according to a modification of the method described in Part A of Example 8. After the reaction was stirred overnight, additional water (100 mL), dichloromethane, and sodium hydrosulfite (20.0 g, 115 mmol) were added, and the reaction was stirred for three additional hours. The organic layer was separated; washed with water (6×), saturated aqueous sodium bicarbonate, and brine; dried over magnesium sulfate; filtered; and concentrated under reduced pressure to provide 40.2 g of ethyl N-(3-aminoquinolin-4-yl)-β-alaninate.

후처리

  1. stirringthe reaction was stirred for three additional hours
  2. customThe organic layer was separated
  3. washwashed with water (6×), saturated aqueous sodium bicarbonate, and brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationand concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9dc6ce1a239343ca94f922e8563efc6a
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697873B2

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