Sodium Carbonate → HCID 9884463, 화합물

HRID 728548

반응식

HRID 728548 반응식
[Na].[NH2:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][C:4]=1C(O)=O.[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2Cl.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.C(O)(=O)C>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2[NH:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][CH:4]=1

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 3045573-Quinolinecarboxylic acid, 4-chloro-8-methoxy-, ethyl esterHCID 5360545SodiumHCID 149896783-Amino-4-methylthiophene-2-carboxylic acid

생성물 1

HCID 9884463HCID 9884463, 화합물수율 31.4%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 702Ethanol용매HCID 1140Toluene용매

실험 절차

The sodium salt of 3-amino-4-methylthiophene-2-carboxylic acid (7.2 g, 0.04 mol) and ethyl 8-methoxy-4-chloroquinoline-3-carboxylate (5.39 g, 0.02 mol) in toluene (75 ml), ethanol (55 ml) and glacial acetic acid (10 ml) were stirred at room temperature for five days. The solvents were removed by evaporation at reduced pressure to give a dark-green slurry. 10% aqueous sodium carbonate was added and the insoluble solid filtered off, washed well with water and dried. This material was crystallised from ethyl acetate (with charcoaling) to give the title compound as pale yellow crystals (2.15 g), m.p. 162°-164°.

후처리

  1. customThe solvents were removed by evaporation at reduced pressure
  2. customto give a dark-green slurry
  3. filtrationthe insoluble solid filtered off
  4. washwashed well with water
  5. customdried
  6. customThis material was crystallised from ethyl acetate (with charcoaling)

출처 및 근거

ORD 기록
ord-124283d1e14b45b483ee120d1584d6ba
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05049567

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