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Sodium hydride → 3-(Pyrazol-1-yloxy)-propylphthalimide

HRID 232021
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반응식

HRID 232021 반응식
[OH:1][N:2]1[CH:6]=[CH:5][CH:4]=[N:3]1.[H-].[Na+].Br[CH2:10][CH2:11][CH2:12][C:13]1[CH:23]=[CH:22][CH:21]=[C:15]2[C:16]([NH:18][C:19](=[O:20])[C:14]=12)=[O:17]>C1(C)C(C)=CC=CC=1>[N:2]1([O:1][CH2:10][CH2:11][CH2:12][C:13]2[CH:23]=[CH:22][CH:21]=[C:15]3[C:16]([NH:18][C:19](=[O:20])[C:14]=23)=[O:17])[CH:6]=[CH:5][CH:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 30167331-hydroxy-1H-pyrazoleHCID 21958088Bromopropylphthalimide

생성물 1

HCID 200307663-(Pyrazol-1-yloxy)-propylphthalimide수율 101.3%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

26 g of 1-hydroxypyrazole are added to a suspension of 10 g of sodium hydride (80 percent strength in oil) in 500 ml of xylene. The mixture is stirred for 1 hour, after which 84 g of 3-bromopropylphthalimide are added and the mixture is refluxed for 2 hours. After cooling, the mixture is filtered, the filtrate is evaporated down, the crystalline residue is suspended in diethyl ether and the product is filtered off under suction. 85 g of the title compound of melting point 116°-118° C. are obtained.

후처리

  1. temperaturethe mixture is refluxed for 2 hours
  2. temperatureAfter cooling
  3. filtrationthe mixture is filtered
  4. customthe filtrate is evaporated down
  5. filtrationthe product is filtered off under suction

출처 및 근거

ORD 기록
ord-6b08d5eaf34d4792b1c35cff93a5f683
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851410

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