Hydrochloric Acid → 4,4'-Dimethoxybibenzyl

HRID 1583558

반응식

HRID 1583558 반응식
[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

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 312751,4-DioxaneHCID 67120Desoxyanisoin

생성물 1

HCID 742614,4'-Dimethoxybibenzyl

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 1140Toluene용매

실험 절차

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 magensium sulfate and concentrated to give 26 g of white waxy solid.

후처리

  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 magensium sulfate
  6. concentrationconcentrated
  7. customto give 26 g of white waxy solid

출처 및 근거

ORD 기록
ord-6415fd7e238c4f79971896db86086bba
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04552876

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