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Potassium Carbonate → ethyl (2Z)-2-(2-amino-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate

HRID 414799
ノート
印刷プレビュー

反応式

HRID 414799 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5](/[C:7](=[N:13]/[OH:14])/[C:8]([O:10][CH2:11][CH3:12])=[O:9])[N:6]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:22]1[CH2:26][CH2:25][NH:24][C:23]1=[O:27]>CS(C)=O.O>[NH2:1][C:2]1[S:3][CH:4]=[C:5](/[C:7](=[N:13]/[O:14][CH:22]2[CH2:26][CH2:25][NH:24][C:23]2=[O:27])/[C:8]([O:10][CH2:11][CH3:12])=[O:9])[N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 6401018Ethyl 2-amino-alpha-(hydroxyimino)thiazol-4-acetateHCID 101034713-Bromopyrrolidin-2-one

生成物 1

HCID 13536830ethyl (2Z)-2-(2-amino-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate収率 86%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒
2 回

実験手順

10.9 g of ethyl (Z)-2-(2-aminothiazol-4-yl)-2-hydroxyiminoacetate are dissolved in 25 ml of dimethylsulfoxide, and a solution of 14 g of anhydrous potassium carbonate in 13 ml of water is added thereto at a temperature of 15° to 20° C. The mixture is stirred at the same temperature for 20 minutes. 10 g of 3-bromo-2-pyrrolidone are added to said mixture at room temperature, and the mixture is stirred at the same temperature for 1.5 hours. 120 ml of water are added to the reaction mixture, and the aqueous mixture is stirred with ice-cooling. Crystalline precipitates are collected by filtration, and the crystals are washed with water and then dried at 40° C. 13 g of ethyl (Z)-2-(2-aminothiazol-4-yl)-2-[(2-pyrrolidon-3yl)oxyimino]acetate are obtained. The physico-chemical properties of this product are identical sith those of the product obtained in Example 2-(3).

後処理

  1. customat a temperature of 15° to 20° C
  2. customat room temperature
  3. stirringthe mixture is stirred at the same temperature for 1.5 hours
  4. stirringthe aqueous mixture is stirred with ice-
  5. temperaturecooling
  6. customCrystalline precipitates
  7. filtrationare collected by filtration
  8. washthe crystals are washed with water
  9. customdried at 40° C

出典と根拠

ORDレコード
ord-6387dcdd172940d5bd1c97f21005facf
出典データセット
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04794186

反応ノート

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