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Dichloromethane → HCID 57447056, 화합물

HRID 2366663
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HRID 2366663 반응식
[CH3:1][C:2]([CH3:23])([CH2:8][NH:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[N:13]=[CH:12][C:11]=1[N+:20]([O-])=O)[C:3]([O:5][CH2:6][CH3:7])=[O:4].S(S([O-])=O)([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+].ClCCl>CC[N+]1C=CC(C2C=C[N+](CC)=CC=2)=CC=1.[Br-].[Br-].O>[NH2:20][C:11]1[CH:12]=[N:13][C:14]2[C:19]([C:10]=1[NH:9][CH2:8][C:2]([CH3:1])([CH3:23])[C:3]([O:5][CH2:6][CH3:7])=[O:4])=[CH:18][CH:17]=[CH:16][CH:15]=2
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참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 24489Sodium DithioniteHCID 57447055HCID 57447055, 화합물

생성물 1

HCID 57447056HCID 57447056, 화합물수율 86.3%

시약·촉매·용매 2

HCID 114742621,1'-Diethyl-4,4'-bipyridinium dibromide
촉매
HCID 962Water용매

실험 절차

Part D A mixture of ethyl 2,2-dimethyl-3-[(3-nitroquinolin-4-yl)amino]propanoate (59 g), sodium hydrosulfite (109 g, 532 mmol), potassium carbonate (103 g, 744 mmol), and ethyl viologen dibromide (0.50 g, 1.3 mmol), dichloromethane (350 mL), and water (350 mL) was stirred overnight at ambient temperature. The aqueous layer was separated and extracted with dichloromethane (100 mL). The combined organic fractions were washes with water (4×75 mL), dried over potassium carbonate, filtered, and concentrated under reduced pressure to provide 46.1 g of ethyl 3-[(3-aminoquinolin-4-yl)amino]-2,2-dimethylpropanoate as a dark oil. Part E

후처리

  1. customThe aqueous layer was separated
  2. extractionextracted with dichloromethane (100 mL)
  3. dry with materialdried over potassium carbonate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-42143018f4c94c41945d5ec0228c68b4
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697873B2

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