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Hydrogen Peroxide → 2-Chloro-5-(oxiranylmethyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide

HRID 1765532
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HRID 1765532 반응식
[Cl:1][C:2]1[CH:21]=[CH:20][C:19]([CH2:22][CH:23]=[CH2:24])=[CH:18][C:3]=1[C:4]([NH:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][CH:10]([CH2:11]3)[CH2:9]1)[CH2:15]2)=[O:5].N1C=CC=N1.[OH:30]O.O>ClCCl.C[Re](=O)(=O)=O>[Cl:1][C:2]1[CH:21]=[CH:20][C:19]([CH2:22][CH:23]2[CH2:24][O:30]2)=[CH:18][C:3]=1[C:4]([NH:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][CH:10]([CH2:11]3)[CH2:9]1)[CH2:15]2)=[O:5]
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참가 물질

7

반응물 4

HCID 784Hydrogen Peroxide2회HCID 962WaterHCID 1048Pyrazole2회HCID 211074042-Chloro-5-(2-propenyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide

생성물 1

HCID 211074132-Chloro-5-(oxiranylmethyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide

시약·촉매·용매 2

HCID 178477782
HCID 178477782, 화합물
촉매
2회
HCID 6344Dichloromethane용매

실험 절차

2-Chloro-5-(2-propenyl)-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide (Example 5a) (9.4 g), pyrazole (0.45 g) and methyltrioxorhenium(VII) (0.40 g) were stirred together in dichloromethane (40 mL) under nitrogen, and hydrogen peroxide (27.5% wt. solution in water, 13 mL) was added dropwise. The reaction was then monitored by HPLC/MS and further portions of pyrazole, methyltrioxorhenium(VII) and hydrogen peroxide were added over a period of 2 days until the reaction mixture consisted of a 1:1 mixture of starting material and product. The mixture was then poured into water (500 mL), extracted into dichloromethane (3×300 mL), washed with 2M aqueous hydrochloric acid (300 mL), brine (300 mL), saturated aqueous sodium thiosulfate (300 mL), dried over anhydrous magnesium sulfate, filtered and concentrated to give an oil. This was purified by column chromatography eluting with 2:1 isohexane/ethyl acetate to give the sub-titled compound (4.71 g).

후처리

  1. additionwere added over a period of 2 days until the reaction mixture
  2. additionconsisted of a 1:1 mixture of starting material and product
  3. extractionextracted into dichloromethane (3×300 mL)
  4. washwashed with 2M aqueous hydrochloric acid (300 mL), brine (300 mL), saturated aqueous sodium thiosulfate (300 mL)
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give an oil
  9. customThis was purified by column chromatography
  10. washeluting with 2:1 isohexane/ethyl acetate

출처 및 근거

ORD 기록
ord-76bf1b84614a4a3387630426baed0903
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07227038B2

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