Sodium Bicarbonate → 2-Methyl-5,6-dihydro-4H-3-thia-1,6-diaza-benzo[e]azulene

HRID 220787ノート

反応式

HRID 220787 の反応式
[CH3:1][C:2]1[S:3][C:4]2[CH2:5][CH2:6][N:7](C(C3C=CC=CC=3)=O)[C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10]=2[N:11]=1.C([O-])(O)=O.[Na+]>Cl>[CH3:1][C:2]1[S:3][C:4]2[CH2:5][CH2:6][NH:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10]=2[N:11]=1

参加物

4

反応物 2

HCID 516892Sodium Bicarbonate2 回HCID 23112323(2-Methyl-4,5-dihydro-3-thia-1,6-diaza-benzo[e]azulen-6-yl)-phenyl-methanone

生成物 1

HCID 231123442-Methyl-5,6-dihydro-4H-3-thia-1,6-diaza-benzo[e]azulene収率 76%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A suspension of (2-methyl-4,5-dihydro-3-thia-1,6-diaza-benzo[e]azulen-6-yl)-phenyl-methanone from Example E7.1 (0.42 g, 1.3 mmol) in 6M hydrochloric acid (45 ml) was heated at reflux for 16 h. The solution was cooled and treated with saturated NaHCO3 (aq) (10 ml). Additional solid NaHCO3 was added until the solution was basic. The mixture was extracted with dichloromethane and the organic extracts were dried and reduced in vacuo to yield the title compound as a yellow oil (0.21 g, 76%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. temperatureThe solution was cooled
  4. extractionThe mixture was extracted with dichloromethane
  5. customthe organic extracts were dried

出典と根拠

ORDレコード
ord-fcb20fc5389b4e96ae1caa1b100418e7
出典データセット
uspto-grants-2012_06
特許番号
US08202858B2

反応ノート

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