Hydrochloric Acid → 3,3-Dimethyl-1-(9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)-2-butanone

HRID 411164ノート

反応式

HRID 411164 の反応式
[CH3:1][C:2]([CH3:23])([CH3:22])[C:3](=[O:21])[CH2:4][N:5]1[CH2:12][CH:11]2[O:13][CH:7]([CH2:8][N:9](C(OC(C)(C)C)=O)[CH2:10]2)[CH2:6]1.Cl.C(#N)C.C([O-])([O-])=O.[K+].[K+]>C(OCC)(=O)C>[CH3:1][C:2]([CH3:23])([CH3:22])[C:3](=[O:21])[CH2:4][N:5]1[CH2:12][CH:11]2[O:13][CH:7]([CH2:8][NH:9][CH2:10]2)[CH2:6]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 18540396Tert-butyl 7-(3,3-dimethyl-2-oxobutyl)-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate

生成物 1

HCID 185403983,3-Dimethyl-1-(9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)-2-butanone収率 86.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

反応条件

温度
0 °C

実験手順

A solution of tert-butyl 7-(3,3-dimethyl-2-oxobutyl)-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylate (from step (i) above; 0.265 g, 0.812 mmol) in ethyl acetate (10 mL) was treated, at 0° C., with ethyl acetate saturated with gaseous hydrochloric acid. The mixture was stirred at 0° C. for 5 h, and then evaporated. Acetonitrile (15 mL) and K2CO3 (1 g, 7.2 mmol) were added, and the mixture was stirred overnight before being filtered and evaporated to yield 0.159 g (86%) of the sub-title compound.

後処理

  1. customevaporated
  2. stirringthe mixture was stirred overnight
  3. filtrationbefore being filtered
  4. customevaporated

出典と根拠

ORDレコード
ord-f45172967c2547d7be0bc3654dffcc31
出典データセット
uspto-grants-2003_05
特許番号
US06559143B1

反応ノート

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