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

HRID 1805972노트

반응식

HRID 1805972 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dac3cef3c5ff4010a7ab817947fa74cc
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354531B2

반응 노트

불러오는 중…