Water → 2-Methyl-3-(3-chloro-2-cyanophenoxy)-1-propene

HRID 233599

反応式

HRID 233599 の反応式
Cl[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:3]=1[C:4]#[N:5].[CH3:11][C:12](=[CH2:15])[CH2:13][OH:14].[OH-].[K+].O>CS(C)=O>[CH3:15][C:12]([CH2:13][O:14][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Cl:10])[C:3]=1[C:4]#[N:5])=[CH2:11]

参加物

6

反応物 4

HCID 962WaterHCID 3031DichlobenilHCID 10557Methallyl alcoholHCID 14797Potassium Hydroxide

生成物 1

HCID 541242722-Methyl-3-(3-chloro-2-cyanophenoxy)-1-propene収率 93.8%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A solution of 30.0 grams (0.174 mole) of 2,6-dichlorobenzonitrile and 14.7 mL (0.174 mole) of 2-methyl-2-propen-1-ol in 200 mL of dimethyl sulfoxide is stirred, and 12.7 grams (0.191 mole) of 85% potassium hydroxide is added portionwise during a 5 minute period. During the addition, the reaction mixture temperature rises from 20° C. to about 35° C. Upon completion of the addition, the reaction mixture is stirred at ambient temperature for about 18 hours. After this time the reaction mixture is poured into 600 mL of water. The mixture is filtered to collect a solid. The solid is washed with water and dried under vacuum, yielding 33.9 grams of 2-methyl-3-(3-chloro-2-cyanophenoxy)-1-propene. The NMR spectrum is consistent with the proposed structure.

後処理

  1. additionDuring the addition
  2. customrises from 20° C. to about 35° C
  3. additionUpon completion of the addition
  4. filtrationThe mixture is filtered
  5. customto collect a solid
  6. washThe solid is washed with water
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-f0700d90ff024e4d9170ebd229069fce
出典データセット
uspto-grants-1997_01
特許番号
US05593998

関連ノート

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