Hydrochloric Acid → HCID 66700868, 화합물

HRID 1253737노트

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HRID 1253737 반응식
[OH:1]S(O)(=O)=O.[CH2:6]([N:13]1[CH2:30][CH2:29][CH2:28][C:16]2([CH:21](C#N)[C:20](=[O:24])N[C:18](=[O:25])[CH:17]2C#N)[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-:31].[Na+].Cl>O>[CH2:6]([N:13]1[CH2:30][CH2:29][CH2:28][C:16]([CH2:17][C:18]([OH:25])=[O:1])([CH2:21][C:20]([OH:24])=[O:31])[CH2:15][CH2:14]1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 667007972,4-Dioxo-9-(phenylmethyl)-3,9-diazaspiro[5.6]dodecane-1,5-dicarbonitrile

생성물 1

HCID 66700868HCID 66700868, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

65% H2SO4 (17.5 ml) was added to a solid powder of 9-benzyl-2,4-dioxo-3,9-diazaspiro[5.6]dodecane-1,5-dicarbonitrile (3.5 g, 10.4 mmol) and the reaction mixture was heated at reflux for 2 h. Then the reaction mixture was cooled to RT, water (6.1 ml) was added and it was again heated at reflux for 20 h. After cooling to 0° C., the reaction mixture was first basified to pH ˜10-12 using 40% NaOH solution and then acidified to pH ˜2-3 using 2 N HCl solution. The solvent was removed under reduced pressure and the residue was dried by azeotropic distillation with benzene. Residual benzene was removed under reduced pressure to afford the dry solid product which was used in the next step without further purification.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 2 h
  3. temperatureit was again heated
  4. temperatureat reflux for 20 h
  5. temperatureAfter cooling to 0° C.
  6. customThe solvent was removed under reduced pressure
  7. dry with materialthe residue was dried by azeotropic distillation with benzene
  8. customResidual benzene was removed under reduced pressure
  9. customto afford the dry solid product which
  10. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-e9489ae95eaf4378af6ff2edacc362d3
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455475B2

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