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1,3-Dichloroacetone → 2-Acetoxymethyl-4-chloromethyl-4-hydroxythiazoline

HRID 1940884
ノート
印刷プレビュー

反応式

HRID 1940884 の反応式
[C:1]([O:4][CH2:5][C:6]([NH2:8])=[S:7])(=[O:3])[CH3:2].[Cl:9][CH2:10][C:11]([CH2:13]Cl)=[O:12].C(=O)(O)[O-].[Na+]>ClCCCl>[C:1]([O:4][CH2:5][C:6]1[S:7][CH2:13][C:11]([CH2:10][Cl:9])([OH:12])[N:8]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 107931,3-DichloroacetoneHCID 516892Sodium BicarbonateHCID 11018908Carbamothioylmethyl acetate

生成物 1

HCID 117908272-Acetoxymethyl-4-chloromethyl-4-hydroxythiazoline収率 92%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 5.33 g of 2-acetoxythioacetamide prepared according to Example 2, 5.21 g of 1,3-dichloroacetone, 6.88 g of sodium bicarbonate and 20 ml of 1,2-dichloroethane was stirred at room temperature for 87 hours. The mixture was filtered to remove insoluble inorganics and concentrated under reduced pressure to an oil. The oil was taken up in 4 mls of 1,2-dichloroethane and 25 mils of cyclohexane added dropwise. The slurry was stirred for 1 hour at 0° C. and then filtered. The precipitate was washed with cyclohexane and dried at room temperature under reduced pressure. The product 2-acetoxymethyl-4-chloromethyl-4-hydroxy-thiazoline was obtained in 92% yield (8.25 g).

後処理

  1. customprepared
  2. filtrationThe mixture was filtered
  3. customto remove insoluble inorganics
  4. concentrationconcentrated under reduced pressure to an oil
  5. addition25 mils of cyclohexane added dropwise
  6. stirringThe slurry was stirred for 1 hour at 0° C.
  7. filtrationfiltered
  8. washThe precipitate was washed with cyclohexane
  9. customdried at room temperature under reduced pressure

出典と根拠

ORDレコード
ord-0f8cf330da5c401ca6ca0ca586526216
出典データセット
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05700945

反応ノート

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