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2,2,6-Trimethyl-4H-1,3-dioxin-4-one → 3-(3-Acetoacetoxypropyl)-5-(4-chlorophenyl)-1-(4-methoxyphenyl) pyrazole

HRID 373492
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인쇄 미리보기

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HRID 373492 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=3)[N:11]=[C:10]([CH2:21][CH2:22][CH2:23][OH:24])[CH:9]=2)=[CH:4][CH:3]=1.[CH3:25][C:26]1[O:32]C(C)(C)O[C:28](=[O:29])[CH:27]=1>>[C:28]([O:24][CH2:23][CH2:22][CH2:21][C:10]1[CH:9]=[C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[N:12]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)[N:11]=1)(=[O:29])[CH2:27][C:26]([CH3:25])=[O:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 793682,2,6-Trimethyl-4H-1,3-dioxin-4-oneHCID 14497416HCID 14497416, 화합물

생성물 1

HCID 179135833-(3-Acetoacetoxypropyl)-5-(4-chlorophenyl)-1-(4-methoxyphenyl) pyrazole수율 80%

실험 절차

5-(4-Chlorophenyl)-3-(3-hydroxypropyl)-1-(4-methoxyphenyl) pyrazole (1.71 g, 0.005 moles) and 2,2,6-trimethyl-1,3-dioxen-4-one (0.71 g, 0.005 moles) were dissolved in 100 ml of xylenes. The solution was stirred under reflux for 16 hours. At that time, the solution was cooled to room temperature, and concentrated in vacuo to a yellow oil. The oil was flash chromatographed on silica gel to afford 59 (1.7 g, 80%) as a pale yellow oil.

후처리

  1. temperatureunder reflux for 16 hours
  2. concentrationconcentrated in vacuo to a yellow oil
custom
chromatographed on silica gel

출처 및 근거

ORD 기록
ord-be504d02f99a4905adaeb22a4e27c7e3
출처 데이터셋
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05164381

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