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

HRID 1789352ノート

反応式

HRID 1789352 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-99a875cbc0914ffc94f639c96f95744e
出典データセット
uspto-grants-1987_08
特許番号
US04689327

反応ノート

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