Acetic Acid → HCID 12898475、化合物

HRID 1579376ノート

反応式

HRID 1579376 の反応式
Br[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:15][C:10]3=[N:11][CH:12]=[CH:13][CH:14]=[C:9]3[C:8](=[O:16])[C:7]=2[CH:17]=1.C1N2CN3CN(C2)CN1C3.C(O)(=[O:30])C.Cl>O>[O:16]=[C:8]1[C:9]2[C:10](=[N:11][CH:12]=[CH:13][CH:14]=2)[O:15][C:6]2[CH:5]=[CH:4][C:3]([CH:2]=[O:30])=[CH:17][C:7]1=2

参加物

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 122742035H-[1]Benzopyrano[2,3-b]pyridin-5-one, 7-(bromomethyl)-

生成物 1

HCID 12898475HCID 12898475、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 50 g of 7-bromomethyl-5-oxo-5H-[1]benzopyrano[2,3-b]pyridine, 48.4 g of hexamethylenetetramine, 167 ml of water and 167 ml of acetic acid is stirred under reflux for 3 hours. To the reaction mixture is added 100 ml of concentrated hydrochloric acid, and the whole mixture is refluxed for 20 minutes. The reaction mixture is diluted with 200 ml of water, and cooled. The crystalline precipitate is filtered off, washed with water, dried, and then recrystallized from dimethylformamide to give 5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-7-carbaldehyde melting at 233-235°C.

後処理

  1. temperatureunder reflux for 3 hours
  2. temperaturethe whole mixture is refluxed for 20 minutes
  3. temperaturecooled
  4. filtrationThe crystalline precipitate is filtered off
  5. washwashed with water
  6. customdried
  7. customrecrystallized from dimethylformamide

出典と根拠

ORDレコード
ord-0f4bfea9a1524446bb412c55e466c363
出典データセット
uspto-grants-1976_01
特許番号
US03931199

反応ノート

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