tert-Butyl piperazine-1-carboxylate → HCID 86686508, compound

HRID 239153Notes

Reaction equation

HRID 239153 reaction equation
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl:14][C:15]1[N:16]=[C:17](Cl)[C:18]2[S:23][CH2:22][CH2:21][C:19]=2[N:20]=1>C(O)C.ClCCl>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:17]2[C:18]3[S:23][CH2:22][CH2:21][C:19]=3[N:20]=[C:15]([Cl:14])[N:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

Participants

5

Reactant 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 457899672,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine

Product 1

HCID 86686508HCID 86686508, compoundYield 96.3%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 6344DichloromethaneSolvent

Conditions

Temperature
60 °C

Procedure

454 mg piperazine-1-carboxylic acid tert-butyl ester in 5 mL ethanol was added to 0.5 g 2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidine in 5 mL dichlormethane. The reaction was stirred 2 h at RT, 3 h at 60° C. and over night at RT. The solvents were removed and water was added to the residue. The precipitate was filtered and dried to give 0.83 g of the desired product.

Workup

  1. customThe solvents were removed
  2. additionwater was added to the residue
  3. filtrationThe precipitate was filtered
  4. customdried

Sources & evidence

ORD record
ord-0e636662478e4814b2734b10dadf6ea2
Source dataset
uspto-grants-2014_02
Patent number
US08642774B2

Reaction notes

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