Potassium Acetate → 5H,6H,7H,8H,9H-pyrido(3,2-b)azepin-6-one

HRID 2220745ノート

反応式

HRID 2220745 の反応式
CC1C=CC(S(O[N:12]=[C:13]2[CH2:22][CH2:21][CH2:20][C:19]3[N:18]=[CH:17][CH:16]=[CH:15][C:14]2=3)(=O)=O)=CC=1.C([O-])(=[O:25])C.[K+]>CCO.O>[N:18]1[C:19]2[CH2:20][CH2:21][CH2:22][C:13](=[O:25])[NH:12][C:14]=2[CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 2

HCID 517044Potassium AcetateHCID 85948845HCID 85948845、化合物

生成物 1

HCID 122830325H,6H,7H,8H,9H-pyrido(3,2-b)azepin-6-one

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A mixture of 1.0 eq of 95 and 2.3 eq of potassium acetate in 70 mL of EtOH and 140 mL of H2O was refluxed for 17 hrs. After cooling to rt and rotary evaporation of the EtOH, the solution was made alkaline with 10 N NaOH. The mixture was extracted with chloroform (3×50 mL). The combined organic extracts were dried over MgSO4 and vacuum filtered. The filtrate was rotary evaporated and dried under vacuum to yield 96.

後処理

  1. temperaturewas refluxed for 17 hrs
  2. customrotary evaporation of the EtOH
  3. extractionThe mixture was extracted with chloroform (3×50 mL)
  4. dry with materialThe combined organic extracts were dried over MgSO4 and vacuum
  5. filtrationfiltered
  6. customThe filtrate was rotary evaporated
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-1274ecf09d6440cdb06d900122c2621f
出典データセット
uspto-grants-2008_08
特許番号
US07417152B2

反応ノート

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