Xanthydrol → ethyl 2-(4-bromo-2-methylbenzoyl)-2-(9H-xanthen-9-yl)acetate

HRID 442798

반응식

HRID 442798 반응식
[CH3:1][C:2]1[CH:15]=[C:14]([Br:16])[CH:13]=[CH:12][C:3]=1[C:4]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].O[CH:18]1[C:31]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[O:25][C:24]2[C:19]1=[CH:20][CH:21]=[CH:22][CH:23]=2>C(O)C.C(O)(=O)C>[Br:16][C:14]1[CH:13]=[CH:12][C:3]([C:4]([CH:6]([CH:18]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:24]=3[O:25][C:26]3[C:31]2=[CH:30][CH:29]=[CH:28][CH:27]=3)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5])=[C:2]([CH3:1])[CH:15]=1

참가 물질

4

반응물 2

HCID 72861XanthydrolHCID 53404613Ethyl 3-(4-bromo-2-methylphenyl)-3-oxopropanoate

생성물 1

HCID 53697250ethyl 2-(4-bromo-2-methylbenzoyl)-2-(9H-xanthen-9-yl)acetate

시약·촉매·용매 1

HCID 18476134Acetic acid ethanol용매

실험 절차

A solution of ethyl 2-methyl-4-bromobenzoylacetate (18.5 g, 65.0 mmol) was heated at 60° C. with 9-hydroxyxanthene (14.2 g, 71.5 mmol) in ethanol-acetic acid (1:1, 200 ml) for 40 h. The product was isolated as in Example 1 (iii), except the aqueous phase was extracted with diethyl ether. The crude product was purified on flash silica eluting with hexane-dichloromethane (3:2 then 1:1) to give ethyl 2-(4-bromo-2-methylbenzoyl)-2-(9H-xanthen-9-yl)acetate as an oil.

후처리

  1. extractionwas extracted with diethyl ether
  2. customThe crude product was purified on flash silica eluting with hexane-dichloromethane (3:2

출처 및 근거

ORD 기록
ord-b115eb2db3a3424eb10f50ab7694ef6f
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891899

연결된 노트

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