Acetic Acid → 2-{2-[2-(4-Phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide

HRID 1789352노트

반응식

HRID 1789352 반응식
[N-:1]=[C:2]=[O:3].[Na+].[C:5]1([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH:26]3[NH:30][CH2:29][CH2:28][S:27]3)[CH2:13][CH2:12]2)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C(O)(=O)C.C(=O)([O-])[O-].[K+].[K+]>O.C(O)C>[C:5]1([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[CH:26]3[N:30]([C:2]([NH2:1])=[O:3])[CH2:29][CH2:28][S:27]3)[CH2:13][CH2:12]2)[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 11430Potassium CarbonateHCID 11051568NaNCOHCID 137680992-{2-[2-(4-Phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine

생성물 1

HCID 137680362-{2-[2-(4-Phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide수율 82.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A solution of 1.07 g of sodium isocyanate in 20 ml of water is added to a solution of 3.03 g of 2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine in 40 ml of ethanol, and 2.46 g of acetic acid are added thereto. The mixture is stirred at room temperature for 2 hours. 200 ml of water are added to the mixture, and the aqueous mixture is made alkaline with potassium carbonate. The aqueous mixture is extracted with ethyl acetate and chloroform, successively. The extracts are combined, washed with water, dried and then concentrated under reduced pressure to remove solvent. The residue is recrystallized from ethyl acetate. 2.78 g of 2-{2-[2-(4-phenylpiperazin-1-yl)ethyloxy]phenyl}thiazolidine-3-carboxamide are obtained. Yield: 82.2%.

후처리

  1. additionare added
  2. extractionThe aqueous mixture is extracted with ethyl acetate and chloroform
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customto remove solvent
  7. customThe residue is recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-99a875cbc0914ffc94f639c96f95744e
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689327

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