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

HRID 1050348ノート

反応式

HRID 1050348 の反応式
[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

参加物

4

反応物 2

HCID 31214Ethyl orthoformateHCID 1185985571279815-28-9

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
140 °C

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-07f6b7946eda4e4398127e5ff5b53256
出典データセット
uspto-grants-2016_07
特許番号
US09382248B2

反応ノート

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