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

HRID 52647

反応式

HRID 52647 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 was stirred, and 12.7 grams (0.191 mole) of 85% potassium hydroxide was added portionwise during a 5 minute period. During the addition, the reaction mixture temperature rose from 20° C. to about 35° C. Upon completion of the addition, the reaction mixture was stirred at ambient temperature for about 18 hours. After this time the reaction mixture was poured into 600 mL of water. The mixture was filtered to collect a solid. The solid was washed with water and dried under vacuum, yielding 33.9 grams of 2-methyl-3-(3-chloro-2-cyanophenoxy)-1-propene. The NMR spectrum was consistent with the proposed structure.

後処理

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

出典と根拠

ORDレコード
ord-cafb03d01c164218a99c58a85408b370
出典データセット
uspto-grants-1997_04
特許番号
US05616718

関連ノート

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