Hydrochloric Acid → 4'-Methoxy(1,1'-biphenyl)-4-carboxylic acid

HRID 1275411

반응식

HRID 1275411 반응식
BrBr.[C:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)=[CH:8][CH:7]=1)(=[O:5])C.S([O-])([O-])=[O:21].[Na+].[Na+].Cl>O.O1CCOCC1>[CH3:19][O:18][C:15]1[CH:16]=[CH:17][C:12]([C:9]2[CH:10]=[CH:11][C:6]([C:3]([OH:5])=[O:21])=[CH:7][CH:8]=2)=[CH:13][CH:14]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 24408BromineHCID 24437Sodium SulfiteHCID 3015571-(4'-Methoxy(1,1'-biphenyl)-4-yl)ethanone

생성물 1

HCID 27595524'-Methoxy(1,1'-biphenyl)-4-carboxylic acid수율 93.1%

시약·촉매·용매 2

HCID 962Water용매3회HCID 312751,4-Dioxane용매2회

반응 조건

온도
0 °C

실험 절차

A solution of 64.7 g (1.61 mol) of soda in 560 ml water is prepared at 0° C. 69.9 g (0.44 mol) of bromine then 260 ml of 1,4-dioxane are added successively. A yellow solution is obtained which is cooled down to 0° C. and which is added over 10 minutes, without exceeding 10° C., to a suspension of 28 g (0.12 mol) of 4'-acetyl-4-methoxybiphenyl in a mixture of 750 ml of 1,4-dioxane and 510 ml water. The reaction medium is agitated for 1 hour at approximately 20° C., a solution of 15.5 g of sodium sulphite in 160 ml water is added and taken to reflux for 10 minutes. 76 ml of concentrated hydrochloric acid is added and the reaction medium is left under agitation whilst being cooled down, for 1 hour. After drying, washing with water and drying at 50° C., 25.5 g of 4'-methoxy-4-biphenyl carboxylic acid is obtained in the form of a white powder (yield: 93%).

후처리

  1. customA yellow solution is obtained which
  2. additionwhich is added over 10 minutes
  3. temperatureto reflux for 10 minutes
  4. waitthe reaction medium is left under agitation
  5. temperaturewhilst being cooled down, for 1 hour
  6. customAfter drying
  7. washwashing with water
  8. customdrying at 50° C.

출처 및 근거

ORD 기록
ord-61b8de6292bf42d3a801a6f444ab5ebe
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06160157

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