1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,4]triazole → 4-[1,2,4]Triazol-1-yl-cyclohexanone

HRID 2099682ノート

反応式

HRID 2099682 の反応式
O1[C:5]2([CH2:10][CH2:9][CH:8]([N:11]3[CH:15]=[N:14][CH:13]=[N:12]3)[CH2:7][CH2:6]2)[O:4]CC1>C1COCC1.Cl>[N:11]1([CH:8]2[CH2:7][CH2:6][C:5](=[O:4])[CH2:10][CH2:9]2)[CH:15]=[N:14][CH:13]=[N:12]1

参加物

4

反応物 1

HCID 574240961-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,4]triazole

生成物 1

HCID 574240934-[1,2,4]Triazol-1-yl-cyclohexanone

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-[1,2,4]triazole (379 mg, 1.81 mmol) was dissolved in a 1:1 mixture of THF and 3N HCl aqueous solution (9 mL). The resulting mixture was stirred at 40° C. for 5 h. Most of the THF was removed under vacuum then the remaining mixture was neutralized using a 3N NaOH aqueous solution until a basic pH was reached. It was extracted with 3 portions of 10 mL of dichloromethane. The organic portions were combined, dried over anhydrous Na2SO4 and concentrated to afford 4-[1,2,4]triazol-1-yl-cyclohexanone as a white waxy solid (257 mg, 86%).

後処理

  1. customMost of the THF was removed under vacuum
  2. extractionIt was extracted with 3 portions of 10 mL of dichloromethane
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-62308a34307f40308177cfff5ef06a89
出典データセット
uspto-grants-2009_08
特許番号
US07569600B2

反応ノート

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