Phosphorus pentachloride → HCID 14878964、化合物

HRID 1084772ノート

反応式

HRID 1084772 の反応式
O[CH2:2][C:3]([CH3:21])([CH3:20])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:23]>C1(C)C(C)=CC=CC=1>[Cl:23][CH2:2][C:3]([CH3:21])([CH3:20])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]=1

参加物

4

反応物 2

HCID 24819Phosphorus pentachlorideHCID 13854275HCID 13854275、化合物

生成物 1

HCID 14878964HCID 14878964、化合物

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

0.5 Gram of 6-phenoxy-2-pyridylmethyl 3-hydroxy-2,2-dimethylpropyl ether was dissolved in 20 ml of dry xylene, and 0.73 g of phosphorus pentachloride was added, followed by heating under reflux for 3 hours. Thereafter, the reaction solution was poured into ice water and extracted with xylene. The xylene layer was washed with water, dried and concentrated. The residue was subjected to column chromatography on silica gel (developing solvent, hexane: ethyl acetate=50:1) to obtain 90 mg of desired 6-phenoxy-2-pyridylmethyl 3-chloro-2,2-dimethylpropyl ether [present compound (1)].

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 3 hours
  3. extractionextracted with xylene
  4. washThe xylene layer was washed with water
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-1d2204eebf4142e3a09b41ac4241052b
出典データセット
uspto-grants-1991_04
特許番号
US05006538

反応ノート

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