Water → HCID 53995533、化合物

HRID 477870ノート

反応式

HRID 477870 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:16][C:17]1[S:18][C:19]([C:23]#[N:24])=[C:20]([NH2:22])[N:21]=1)[CH2:13][CH2:14][CH3:15].C(=O)(O)[O-].[Na+].[OH2:30]>C(Cl)Cl>[CH2:12]([S:16]([C:17]1[S:18][C:19]([C:23]#[N:24])=[C:20]([NH2:22])[N:21]=1)(=[O:9])=[O:30])[CH2:13][CH2:14][CH3:15]

参加物

6

反応物 4

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 542743064-Amino-2-(butylsulfanyl)-1,3-thiazole-5-carbonitrile

生成物 1

HCID 53995533HCID 53995533、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

9.0 g of 85% m-chloroperbenzoic acid are added in portions to a solution of 4.26 g of 2-n-butylthio-4-amino-5-cyanothiazole in 200 ml of methylene chloride, while stirring and at room temperature. After stirring overnight at room temperature an excess of sodium bicarbonate in water is added and the solution is stirred for one hour. The organic layer is separated, washed with water, dried, filtered and diluted with isopropanol. After distilling off a part of the methylene chloride the desired product crystallises: yield 4.34 g; melting-point 150°-152° C.; TLC: Rf (CH2Cl2) 0.05.

後処理

  1. additionis added
  2. stirringthe solution is stirred for one hour
  3. customThe organic layer is separated
  4. washwashed with water
  5. customdried
  6. filtrationfiltered
  7. additiondiluted with isopropanol
  8. distillationAfter distilling off a part of the methylene chloride the desired product
  9. customcrystallises
  10. custommelting-point 150°-152° C.

出典と根拠

ORDレコード
ord-3d5b85b8c45244cab7d27dbfacd02146
出典データセット
uspto-grants-1989_12
特許番号
US04889863

反応ノート

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