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Acetic acid, 2-(2-chloroethyl)thio-, methyl ester → HCID 20133529、化合物

HRID 986294
ノート
印刷プレビュー

反応式

HRID 986294 の反応式
ClC1C=C(C=CC=1)C(OO)=[O:6].[Cl:12][CH2:13][CH2:14][S:15][CH2:16][C:17]([O:19][CH3:20])=[O:18]>C(Cl)Cl>[Cl:12][CH2:13][CH2:14][S:15]([CH2:16][C:17]([O:19][CH3:20])=[O:18])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 51933Acetic acid, 2-(2-chloroethyl)thio-, methyl esterHCID 70297m-Chloroperbenzoic acid

生成物 1

HCID 20133529HCID 20133529、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

3-Chloro-peroxybenzoic acid (81%, 4.7 g, 0.022 mole) was added to the title compound of Example 10 (3.7 g, 0.022 mole) in cold (5° C.) methylene chloride (75 ml) stirred for 30 minutes and cooled in a refrigerator for 48 hours. After removing the solid by filtration, a saturated solution of sodium thiosulfate (30 ml) was added and the mixture stirred for 15 minutes. The layers were separated and the organic layer was washed with saturated sodium bicarbonate (2×50 ml), dried over sodium sulfate, filtered and the solvent removed on a rotary evaporator. The residue was crystallized from ethyl acetate and hexane to give a white solid which was identified as the title compound by its NMR and IR spectra.

後処理

  1. temperaturecooled in a refrigerator for 48 hours
  2. customAfter removing the solid
  3. filtrationby filtration
  4. additiona saturated solution of sodium thiosulfate (30 ml) was added
  5. stirringthe mixture stirred for 15 minutes
  6. customThe layers were separated
  7. washthe organic layer was washed with saturated sodium bicarbonate (2×50 ml)
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. customthe solvent removed on a rotary evaporator
  11. customThe residue was crystallized from ethyl acetate and hexane
  12. customto give a white solid which

出典と根拠

ORDレコード
ord-6a1f9a8dbdb8459ca46b34d8bd58e177
出典データセット
uspto-grants-1987_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04711903

反応ノート

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