Diethyl Ether → Sulisobenzone

HRID 1460856

반응식

HRID 1460856 반응식
[OH:1][C:2]1[CH:15]=[C:14]([O:16][CH3:17])[CH:13]=[CH:12][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:5].Cl[S:19]([OH:22])(=[O:21])=[O:20].CCOCC>C(OC)(=O)C1C(=CC=CC=1)C(OC)=O>[CH3:17][O:16][C:14]1[CH:15]=[C:2]([OH:1])[C:3]([C:4]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[O:5])=[CH:12][C:13]=1[S:19]([OH:22])(=[O:21])=[O:20]

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 46322-Hydroxy-4-methoxybenzophenoneHCID 24638Chlorosulfonic acid

생성물 1

HCID 19988Sulisobenzone

시약·촉매·용매 1

HCID 8554Dimethyl Phthalate용매

실험 절차

11.4 g of 2-hydroxy-4-methoxybenzophenone were dissolved in 30 ml of dimethyl phthalate at 80° C., and 3.5 ml of chlorosulfonic acid were added dropwise at this temperature. Stirring was carried out for a further 4 hours at 80° C., the mixture was cooled to room temperature and 25 ml of ether were added to the solution. The precipitate was filtered off under suction, washed with ether and hexane and dried under reduced pressure at 30° C. 10 g of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid of melting point 112°-114° C. were obtained (water content 7.7%).

후처리

  1. filtrationThe precipitate was filtered off under suction
  2. washwashed with ether and hexane
  3. customdried under reduced pressure at 30° C

출처 및 근거

ORD 기록
ord-fcebcd7a640d4fd183927000023c6b61
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05072034

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