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

HRID 220787노트

반응식

HRID 220787 반응식
[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

참가 물질

4

반응물 2

HCID 516892Sodium Bicarbonate2회HCID 23112323(2-Methyl-4,5-dihydro-3-thia-1,6-diaza-benzo[e]azulen-6-yl)-phenyl-methanone

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-fcb20fc5389b4e96ae1caa1b100418e7
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202858B2

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