Chloromethyl Methyl Ether → 3-Chloro-4-methoxymethoxy-5-methyl-1-benzoyloxybenzene

HRID 1356979ノート

反応式

HRID 1356979 の反応式
[C:1]([O:9][C:10]1[CH:15]=[C:14]([CH3:16])[C:13]([OH:17])=[C:12]([Cl:18])[CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:19][O:20][CH2:21]Cl.C(N(C(C)C)C(C)C)C>C(Cl)(Cl)Cl>[Cl:18][C:12]1[CH:11]=[C:10]([O:9][C:1](=[O:8])[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:15]=[C:14]([CH3:16])[C:13]=1[O:17][CH2:19][O:20][CH3:21]

参加物

5

反応物 3

HCID 7864Chloromethyl Methyl EtherHCID 81531DiisopropylethylamineHCID 185045884-Benzoyloxy-2-chloro-6-methylphenol

生成物 1

HCID 185046333-Chloro-4-methoxymethoxy-5-methyl-1-benzoyloxybenzene収率 96%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

Then, 25 g of 4-benzoyloxy-2-chloro-6-methylphenol was dissolved in 250 ml of chloroform, to which 12 g of chloromethyl methyl ether was added, while stirring at 0° C., and 21 g of N-ethyldiisopropylamine was added dropwise. After heating under reflux for 1 hour, the chloroform layer was washed with water, and concentrated. The residue was subjected to silica gel chromatography, which afforded 27.4 g of 3-chloro-4-methoxymethoxy-5-methyl-1-benzoyloxybenzene (96% yield).

後処理

  1. additionwas added
  2. temperatureAfter heating
  3. temperatureunder reflux for 1 hour
  4. washthe chloroform layer was washed with water
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-af5265db46de4142a39df0c85568de97
出典データセット
uspto-grants-2003_07
特許番号
US06589914B2

反応ノート

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