Ethyl orthoformate → Pyrido[4,3-d]pyrimidin-4(3H)-one, 7-chloro-

HRID 1050348노트

반응식

HRID 1050348 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[CH:4][C:3]=1[C:9]([NH2:11])=[O:10].[CH2:12](OC(OCC)OCC)C>C(OCC)C>[Cl:8][C:6]1[N:5]=[CH:4][C:3]2[C:9](=[O:10])[NH:11][CH:12]=[N:1][C:2]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 31214Ethyl orthoformateHCID 1185985571279815-28-9

생성물 1

HCID 136980669Pyrido[4,3-d]pyrimidin-4(3H)-one, 7-chloro-

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
140 °C

실험 절차

4-Amino-6-chloro-pyridine-3-carboxamide (2, 4.5 g, 26.23 mmol) was added to a pressure tube and triethylorthoformate (30 mL) was added. The reaction vessel was sealed and heated to 140° C. for 11 h. After the cyclization was complete, the reaction mixture was concentrated under reduced pressure, and to the solid obtained was added diethyl ether. The solid was filtered, washed with diethyl ether and dried in vacuum to afford 7-chloro-3H-pyrido[4,3-d]pyrimidin-4-one (3) as brown solid. MS (ESI) m/z 181.90 [M+1]+.

후처리

  1. customThe reaction vessel was sealed
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customto the solid obtained
  4. filtrationThe solid was filtered
  5. washwashed with diethyl ether
  6. customdried in vacuum

출처 및 근거

ORD 기록
ord-07f6b7946eda4e4398127e5ff5b53256
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09382248B2

반응 노트

불러오는 중…