Hydrochloric Acid → 4,4'-Dimethoxybibenzyl

HRID 979066

反応式

HRID 979066 の反応式
[C:1]1([C:9]([CH2:11][C:12]2[CH:19]=[CH:18][C:15]([O:16][CH3:17])=[CH:14][CH:13]=2)=O)[CH:8]=[CH:7][C:4]([O:5][CH3:6])=[CH:3][CH:2]=1.O1CCOCC1.Cl>[Zn].C1(C)C=CC=CC=1>[CH3:17][O:16][C:15]1[CH:14]=[CH:13][C:12]([CH2:11][CH2:9][C:1]2[CH:2]=[CH:3][C:4]([O:5][CH3:6])=[CH:7][CH:8]=2)=[CH:19][CH:18]=1

参加物

6

反応物 3

HCID 313Hydrochloric Acid2 回HCID 312751,4-DioxaneHCID 67120Desoxyanisoin

生成物 1

HCID 742614,4'-Dimethoxybibenzyl

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 1140Toluene溶媒

実験手順

A mixture of 60 g of desoxyanisoin, 120 g of amalgamated zinc, 200 ml of dioxane, 100 ml of toluene and 200 ml of concentrated hydrochloric acid was refluxed for 24 hours. Another 50 ml of concentrated hydrochloric acid was added after the first 6 hours. The reaction mixture was cooled to room temperature and the organic layer was separated and mixed with 300 ml of ethyl acetate. It was washed with water, dried over anhydrous magnesium sulfate and concentrated to give 26 g of white waxy solid.

後処理

  1. temperaturewas refluxed for 24 hours
  2. customthe organic layer was separated
  3. additionmixed with 300 ml of ethyl acetate
  4. washIt was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto give 26 g of white waxy solid

出典と根拠

ORDレコード
ord-ad30e23285dd48ffb981e09dea068b82
出典データセット
uspto-grants-1987_05
特許番号
US04666909

関連ノート

読み込み中…