Diethyl Ether → Sulisobenzone

HRID 1460856

反応式

HRID 1460856 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 19988Sulisobenzone

試薬・触媒・溶媒 1

HCID 8554Dimethyl Phthalate溶媒

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-fcebcd7a640d4fd183927000023c6b61
出典データセット
uspto-grants-1991_12
特許番号
US05072034

関連ノート

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