4-(2-Chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-carboxy-2-methoxyphenyl)-N-propylamino]thiazole → 4-(2-Chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-acetyl-2-methoxyphenyl)-N-propylamino]thiazole

HRID 1698869

반응식

HRID 1698869 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[N:11]=[C:12]([N:16]([C:20]2[CH:25]=[C:24]([C:26](O)=[O:27])[CH:23]=[CH:22][C:21]=2[O:29][CH3:30])[CH2:17][CH2:18][CH3:19])[S:13][C:14]=1[CH3:15].[CH3:31][Li]>C(OCC)C.C(OCC)(=O)C>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[N:11]=[C:12]([N:16]([C:20]2[CH:25]=[C:24]([C:26](=[O:27])[CH3:31])[CH:23]=[CH:22][C:21]=2[O:29][CH3:30])[CH2:17][CH2:18][CH3:19])[S:13][C:14]=1[CH3:15]

참가 물질

5

반응물 2

HCID 183222624-(2-Chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-carboxy-2-methoxyphenyl)-N-propylamino]thiazoleHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 183222784-(2-Chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-acetyl-2-methoxyphenyl)-N-propylamino]thiazole

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매

실험 절차

At 0° C., under an inert atmosphere, 2 g of 4-(2-chloro-4-methoxyphenyl)-5-methyl-2-[N-(5-carboxy-2-methoxyphenyl)-N-propylamino]thiazole are dissolved in 30 ml of diethyl ether. Methyllithium (3 equivalents) is slowly added to the ethereal solution. When the addition is complete, the reaction mixture is brought to room temperature. After 2 hours, it is diluted with ethyl acetate and then hydrolyzed. The organic phase is washed with water and then dried over sodium sulphate. After evaporation, the residue is purified on a silica gel. The expected product is obtained in the form of a powder; m.p.=50° C.

후처리

  1. additionWhen the addition
  2. customis brought to room temperature
  3. washThe organic phase is washed with water
  4. dry with materialdried over sodium sulphate
  5. customAfter evaporation
  6. customthe residue is purified on a silica gel

출처 및 근거

ORD 기록
ord-a3d841618b7445379ce7ea643665f5d8
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06344470B1

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