Sodium Hydroxide → HCID 135715026, compound

HRID 273788Notes

Reaction equation

HRID 273788 reaction equation
Cl[CH2:2][C:3]1[N:12]2[N:13]=[CH:14][CH:15]=[C:11]2[C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[N:4]=1.[OH-:16].[Na+]>O1CCOCC1>[CH:15]1[CH:14]=[N:13][N:12]2[C:11]=1[C:10]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:4][C:2](=[O:16])[CH2:3]2

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 20093956HCID 20093956, compound

Product 1

HCID 135715026HCID 135715026, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

3.1. A solution of 11.4 g of 5-(chloromethyl)pyrazolo[1,5-c]quinazoline in 160 ml of dioxan is added dropwise within 15 min. to a mixture of 130 ml of 1N aqueous sodium hydroxide solution and 130 ml of dioxan cooled to 0° to 5° C. The cooling is removed and the mixture is stirred at room temperature for 2.5 h. Then, the reaction mixture is poured into 600 ml of saturated aqueous sodium chloride solution and extracted four times with dichloromethane. The dichloromethane extracts are evaporated in a vacuum. The residue (5.4 g) is crystallized from dichloromethane/diethyl ether. There are obtained 4.15 g of 5H-pyrazolo[1,5-d][1,4]benzodiazepin-6(7H)-one of m.p. 236°-240° C.

Workup

  1. temperaturecooled to 0° to 5° C
  2. customThe cooling is removed
  3. additionThen, the reaction mixture is poured into 600 ml of saturated aqueous sodium chloride solution
  4. extractionextracted four times with dichloromethane
  5. customThe dichloromethane extracts are evaporated in a vacuum
  6. customThe residue (5.4 g) is crystallized from dichloromethane/diethyl ether

Sources & evidence

ORD record
ord-40dec598b96a42ed9a3acd3bed952abf
Source dataset
uspto-grants-1995_02
Patent number
US05387585

Reaction notes

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