Water → HCID 21019138、化合物

HRID 1744722ノート

反応式

HRID 1744722 の反応式
[CH3:1][C:2]1([CH3:17])[CH2:7][O:6][P:5](=[O:16])([O:8][CH2:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH:12]=[CH:11]2)[O:4][CH2:3]1.C(OO)(=[O:20])C.O>C(Cl)Cl>[CH3:1][C:2]1([CH3:17])[CH2:3][O:4][P:5](=[O:16])([O:8][CH2:9][CH:10]2[CH2:15][CH2:14][CH:13]3[CH:12]([O:20]3)[CH2:11]2)[O:6][CH2:7]1

参加物

5

反応物 3

HCID 962WaterHCID 6585Peracetic AcidHCID 22222978HCID 22222978、化合物

生成物 1

HCID 21019138HCID 21019138、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A 500 mL round bottom flask equipped with a stirrer bar was charged with 15.5 g (0.058 mol) 3-(5,5-dimethyl-2-oxo-1,3,2-dioxaphosphorinanoxymethyl)-1-cyclohexene, and 100 mL of methylene chloride. Peracetic acid (13.76 g, 35 wt. % in acetic acid; 0.058 mol) in methylene chloride (60 mL) was added dropwise to above mixture over 20 min. in an ice bath. After the above mixture was reacted at room temperature overnight, 100 mL of water was added to above reaction mixture, the water layer was extracted with methylene chloride (2×100 mL), the organic layer was combined, and washed with saturated sodium carbonate solution (2×100 mL), then with water (2×100 mL), dried with sodium sulfate. The solvent was evaporated and the residue distilled to give pure product.

後処理

  1. customA 500 mL round bottom flask equipped with a stirrer bar
  2. customAfter the above mixture was reacted at room temperature overnight
  3. extractionthe water layer was extracted with methylene chloride (2×100 mL)
  4. washwashed with saturated sodium carbonate solution (2×100 mL)
  5. dry with materialwith water (2×100 mL), dried with sodium sulfate
  6. customThe solvent was evaporated
  7. distillationthe residue distilled
  8. customto give pure product

出典と根拠

ORDレコード
ord-d97466e4e19b4512a38601257b1954cc
出典データセット
uspto-grants-2006_03
特許番号
US07018559B2

反応ノート

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