Acetic Acid → HCID 13229174、化合物

HRID 1579379ノート

反応式

HRID 1579379 の反応式
Cl[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[CH2:8][C:7]=2[CH:16]=1.C1N2CN3CN(C2)CN1C3.C(O)(=[O:29])C.Cl>O>[N:11]1[CH:12]=[CH:13][CH:14]=[C:9]2[CH2:8][C:7]3[CH:16]=[C:3]([CH:2]=[O:29])[CH:4]=[CH:5][C:6]=3[O:15][C:10]=12

参加物

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 12274208HCID 12274208、化合物

生成物 1

HCID 13229174HCID 13229174、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 52 g of 7-chloromethyl-5H-[1]benzopyrano[2,3-b]pyridine, 63 g of hexamethylenetetramine, 160 ml of water and 160 ml of acetic acid is stirred under reflux for 3 hours. To the reaction mixture is added 80 ml of concentrated hydrochloric acid, and the whole mixture is refluxed for 20 minutes, then diluted with 200 ml of water, and cooled. The crystalline precipitate is filtered off, washed with water, dried, and then recrystallized from dioxane to give 5H-[1]benzopyrano[2,3-b]pyridine-7-carbaldehyde melting at 171°-173°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 dioxane

出典と根拠

ORDレコード
ord-b2b560df89df427fb3318e78da2a6ef1
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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