Acetic Acid Mixture with Hydrobromic Acid → 1-(2-Bromomethyl-3-cyclopropylphenyl)-4-methyl-1,4-dihydrotetrazol-5-one

HRID 628493노트

반응식

HRID 628493 반응식
CO[CH2:3][C:4]1[C:9]([CH:10]2[CH2:12][CH2:11]2)=[CH:8][CH:7]=[CH:6][C:5]=1[N:13]1[C:17](=[O:18])[N:16]([CH3:19])[N:15]=[N:14]1.[BrH:20].C(O)(=O)C>C(O)(=O)C>[Br:20][CH2:3][C:4]1[C:9]([CH:10]2[CH2:12][CH2:11]2)=[CH:8][CH:7]=[CH:6][C:5]=1[N:13]1[C:17](=[O:18])[N:16]([CH3:19])[N:15]=[N:14]1

참가 물질

4

반응물 2

HCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 898812581-(2-Methoxymethyl-3-cyclopropylphenyl)-4-methyl-1,4-dihydrotetraz ol-5-one

생성물 1

HCID 898757781-(2-Bromomethyl-3-cyclopropylphenyl)-4-methyl-1,4-dihydrotetrazol-5-one

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
65 °C

실험 절차

A mixture of 1-(2-methoxymethyl-3-cyclopropylphenyl)-4-methyl-1,4-dihydrotetrazole-5-one (described in Reference Preparation example 7) 26.0 g, acetic acid 40 ml and 25% hydrogen bromide-acetic acid solution 40 ml was stirred at 65° C. for two hours. To the reaction mixture was added saturated saline, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium bicarbonate solution and was dried over anhydrous sodium sulfate. The mixture was concentrated under reduced pressure to give 1-(2-bromomethyl-3-cyclopropylphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 30.8 g.

후처리

  1. additionTo the reaction mixture was added saturated saline
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with aqueous saturated sodium bicarbonate solution
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. concentrationThe mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0d7493253b994d529661e678f9b24929
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09314023B2

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