Propylamine → (2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)propylamine

HRID 1805972ノート

反応式

HRID 1805972 の反応式
[Cl:1][C:2]1[N:3]=[C:4](Cl)[C:5]2[S:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[CH2:12]([NH2:15])[CH2:13][CH3:14].C(N(C(C)C)C(C)C)C>O1CCCC1>[Cl:1][C:2]1[N:3]=[C:4]([CH2:14][CH2:13][CH2:12][NH2:15])[C:5]2[S:10][CH2:9][CH2:8][C:6]=2[N:7]=1

参加物

5

反応物 3

HCID 7852PropylamineHCID 81531DiisopropylethylamineHCID 127128322,4-Dichlorothieno[3,2-d]pyrimidine

生成物 1

HCID 86632801(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)propylamine収率 86.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

10.4 g (50.2 mmol) of 2,4-dichlorothieno[3,2-d]pyrimidine (VII), 8.2 mL (100 mmol) of N-propylamine, and 17.5 mL (100 mmol) of N-ethyldiisopropylamine are placed in 100 mL of tetrahydrofuran and stirred for 20 hours at ambient temperature. The suspension is filtered, the filtrate is concentrated by evaporation. The residue is combined with 100 mL of water and treated in the ultrasound bath. Solid substance is suction filtered, dried, and stirred with 50 mL of petroleum ether. 10.0 g of the product VIII (86%) is obtained as a powder.

後処理

  1. filtrationThe suspension is filtered
  2. concentrationthe filtrate is concentrated by evaporation
  3. additiontreated in the ultrasound bath
  4. filtrationfiltered
  5. customdried
  6. stirringstirred with 50 mL of petroleum ether

出典と根拠

ORDレコード
ord-dac3cef3c5ff4010a7ab817947fa74cc
出典データセット
uspto-grants-2013_01
特許番号
US08354531B2

反応ノート

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