Ammonia → HCID 21266002, compound

HRID 566276Notes

Reaction equation

HRID 566276 reaction equation
[NH3:1].[C:2]1([C:8]2[C:9]3[S:32][CH:31]=[CH:30][C:10]=3[N:11]=[C:12](OP(N3CCOCC3)(N3CCOCC3)=O)[CH2:13][N:14]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>>[C:2]1([C:8]2[C:9]3[S:32][CH:31]=[CH:30][C:10]=3[N:11]=[C:12]([NH2:1])[CH2:13][N:14]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

3

Reactant 2

HCID 222AmmoniaHCID 53773170HCID 53773170, compound

Product 1

HCID 21266002HCID 21266002, compound

Procedure

Gaseous ammonia was conducted into a solution of 14.4 g of dimorpholin-4-yl-phosphinic acid (5-phenyl-3H-thieno[3,2-e][1,4]-diazepin-2-yl) ester at room temperature while stirring until the starting product had reacted completely. After removal of the solvent in a vacuum the residue was extracted with dichloromethane/water in the presence of a small amount of methanol. The aqueous phase was washed several times with dichloromethane, the dichloromethane extracts were dried with sodium sulphate, filtered and evaporated in a vacuum. The residue was suspended in dichloromethane and stirred for 0.5 h. There were obtained 2.9 g of crude 5-phenyl-3H-thieno[3,2-e][1,4]diazepin-2-ylamine which was used without further purification as the starting product for the step described below.

Workup

  1. customhad reacted completely
  2. customAfter removal of the solvent in a vacuum the residue
  3. extractionwas extracted with dichloromethane/water in the presence of a small amount of methanol
  4. washThe aqueous phase was washed several times with dichloromethane
  5. dry with materialthe dichloromethane extracts were dried with sodium sulphate
  6. filtrationfiltered
  7. customevaporated in a vacuum
  8. stirringstirred for 0.5 h

Sources & evidence

ORD record
ord-6150b30ff5874418987700fdd58e80d6
Source dataset
uspto-grants-2001_01
Patent number
US06174881B1

Reaction notes

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