1,4-Dioxane hydrochloride → HCID 69076795, compound

HRID 225480Notes

Reaction equation

HRID 225480 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:15]3[S:31][CH:30]=[CH:29][C:16]=3[N:17]=[C:18]([C:20]3[CH:25]=[C:24]([F:26])[C:23]([Cl:27])=[CH:22][C:21]=3[F:28])[N:19]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:32].O1CCOCC1>CCOC(C)=O>[ClH:27].[ClH:32].[Cl:27][C:23]1[C:24]([F:26])=[CH:25][C:20]([C:18]2[N:19]=[C:14]([N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)[C:15]3[S:31][CH:30]=[CH:29][C:16]=3[N:17]=2)=[C:21]([F:28])[CH:22]=1

Participants

4

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 69077884HCID 69077884, compound

Product 1

HCID 69076795HCID 69076795, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

A mixture of 1.16 g of 1-tert-butoxycarbonyl-4-[2-(4-chloro-2,5-difluorophenyl)thieno[3,2-d]pyrimidine-4-yl]piperazine and 10 ml of 4M HCl-dioxane solution was stirred for two days at room temperature. 10 ml of EtOAc was added to the reaction mixture. After the precipitate was filtered and washed with EtOAc, it was dried under reduced pressure to give 1.17 g of 2-(4-chloro-2,5-difluorophenyl)-4-piperazine-1-ylthieno[3,2-d]pyrimidine dihydrochloride.

Workup

  1. filtrationAfter the precipitate was filtered
  2. washwashed with EtOAc, it
  3. customwas dried under reduced pressure

Sources & evidence

ORD record
ord-0289d2e9010e469c862237d64ac49e2d
Source dataset
uspto-grants-2009_07
Patent number
US07557112B2

Reaction notes

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