Water → Methyl 2-(4-chloromethylphenoxy)propionate

HRID 426434ノート

反応式

HRID 426434 の反応式
O[CH2:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][CH:8]([CH3:13])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1.S(Cl)([Cl:18])=O.O>CN(C)P(=O)(N(C)C)N(C)C>[Cl:18][CH2:2][C:3]1[CH:15]=[CH:14][C:6]([O:7][CH:8]([CH3:13])[C:9]([O:11][CH3:12])=[O:10])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 962WaterHCID 24386Thionyl ChlorideHCID 18759642Methyl 2-(4-hydroxymethylphenoxy)propionate

生成物 1

HCID 18981037Methyl 2-(4-chloromethylphenoxy)propionate

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

反応条件

温度
-10 °C

実験手順

12 gm (0.058 mol) of methyl 2-(4-hydroxymethyl-phenoxy)-propionate were dissolved in 60 ml of hexamethylphosphoric acid triamide, the solution was cooled to -10° C., and 4.4 ml (0.06 mol) of thionyl chloride were added dropwise thereto. The resulting mixture was stirred for 30 minutes at 0° C. and then for one hour at 10° C., and subsequently poured into water. The aqueous mixture was extracted with ether, and the extract solution was washed with water, sodium bicarbonate solution and again with water, and dried. The ether was subsequently removed in vacuo at room temperature, leaving methyl 2-(4-chloromethyl-phenoxy)-propionate as a residue.

後処理

  1. waitfor one hour at 10° C.
  2. extractionThe aqueous mixture was extracted with ether
  3. washthe extract solution was washed with water, sodium bicarbonate solution and again with water
  4. customdried
  5. customThe ether was subsequently removed in vacuo at room temperature

出典と根拠

ORDレコード
ord-e85283782f1743b38c530220aabbb815
出典データセット
uspto-grants-1979_10
特許番号
US04169720

反応ノート

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