Benzene → 3-Chloromethyl-4-(4-methyl-phenoxy)-toluene

HRID 372418ノート

反応式

HRID 372418 の反応式
S(Cl)([Cl:3])=O.[CH3:5][C:6]1[CH:21]=[CH:20][C:9]([O:10][C:11]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:12]=2[CH2:13]O)=[CH:8][CH:7]=1.N1C=CC=CC=1.C1C=CC=CC=1>O>[Cl:3][CH2:13][C:12]1[CH:15]=[C:16]([CH3:19])[CH:17]=[CH:18][C:11]=1[O:10][C:9]1[CH:20]=[CH:21][C:6]([CH3:5])=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 241BenzeneHCID 1049PyridineHCID 24386Thionyl ChlorideHCID 54261585HCID 54261585、化合物

生成物 1

HCID 227679253-Chloromethyl-4-(4-methyl-phenoxy)-toluene

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

36.5 Ml. of thionyl chloride are added dropwise at 10°-15° C. with stirring and cooling with ice to a solution of 110 g. of 2-(4-methyl-phenoxy)-5-methylbenzyl alcohol in 78 ml. of pyridine. The mixture is stirred for an additional 1 hour at 10° C. and then diluted with 200 ml. of benzene. Then, 200 ml. of water are carefully added dropwise with ice-cooling. The aqueous phase is separated and the organic phase washed successively with dilute hydrochloric acid, water and saturated sodium bicarbonate solution. The aqueous phases are each extracted once more with benzene. The combined benzene extracts are dried over sodium sulfate and evaporated to dryness in vacuo and there is obtained 3-chloromethyl-4-(4-methyl-phenoxy)-toluene as an oil.

後処理

  1. temperaturecooling with ice to a solution of 110 g
  2. stirringThe mixture is stirred for an additional 1 hour at 10° C.
  3. additiondiluted with 200 ml
  4. temperaturecooling
  5. customThe aqueous phase is separated
  6. washthe organic phase washed successively with dilute hydrochloric acid, water and saturated sodium bicarbonate solution
  7. extractioneach extracted once more with benzene
  8. dry with materialThe combined benzene extracts are dried over sodium sulfate
  9. customevaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-977ace92b44f41078b7cdb6ed70f60ee
出典データセット
uspto-grants-1978_05
特許番号
US04091023

反応ノート

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