Sodium Carbonate → HCID 9884463、化合物

HRID 728548

反応式

HRID 728548 の反応式
[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

参加物

8

反応物 4

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

生成物 1

HCID 9884463HCID 9884463、化合物収率 31.4%

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 1140Toluene溶媒

実験手順

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°.

後処理

  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)

出典と根拠

ORDレコード
ord-124283d1e14b45b483ee120d1584d6ba
出典データセット
uspto-grants-1991_09
特許番号
US05049567

関連ノート

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