4-Chloro-2-(4-phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidine → (2-Piperazin-1-yl-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)propylamine

HRID 2240110ノート

反応式

HRID 2240110 の反応式
Cl[C:2]1[C:3]2[S:22][CH2:21][CH2:20][C:4]=2[N:5]=[C:6]([N:8]2[CH2:13][CH2:12][N:11](C3C=CC=CC=3)[CH2:10][CH2:9]2)[N:7]=1.[CH:23]1([NH:29]C2C3SCCC=3N=C(N3CCN(C4C=CC(C(OCC)=O)=CC=4)CC3)N=2)CCC[CH2:25][CH2:24]1>O1CCOCC1>[N:8]1([C:6]2[N:7]=[C:2]([CH2:25][CH2:24][CH2:23][NH2:29])[C:3]3[S:22][CH2:21][CH2:20][C:4]=3[N:5]=2)[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1

参加物

4

反応物 2

HCID 866162644-Chloro-2-(4-phenylpiperazin-1-yl)-6,7-dihydrothieno[3,2-d]pyrimidineHCID 86616266Ethyl 4-[4-(4-cyclohexylamino-6,7-dihydrothieno[3,2-d]pyrimidin-2-yl)piperazin-1-yl]benzoate

生成物 1

HCID 68438559(2-Piperazin-1-yl-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)propylamine収率 80%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

1.0 g (4.4 mmol) of (2-chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)propylamine (V) and 1.9 g (21.8 mmol) of piperazine (VI) are placed in 10 mL of dioxane, then reacted for 0.7 hours at 150° C. in the microwave. Then the reaction mixture is extracted with water and ethyl acetate, and the organic phase is dried and evaporated to dryness. The residue is triturated with petroleum ether and suction filtered. 0.97 g of product VII (80%) is obtained as a powder.

後処理

  1. customreacted for 0.7 hours at 150° C. in the microwave
  2. extractionThen the reaction mixture is extracted with water and ethyl acetate
  3. customthe organic phase is dried
  4. customevaporated to dryness
  5. customThe residue is triturated with petroleum ether and suction
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-45329cac83554f5688eb1891b6e6837e
出典データセット
uspto-grants-2010_05
特許番号
US07723341B2

反応ノート

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