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

HRID 628493ノート

反応式

HRID 628493 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
65 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0d7493253b994d529661e678f9b24929
出典データセット
uspto-grants-2016_04
特許番号
US09314023B2

反応ノート

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