Acetic Acid → HCID 12898475, 화합물

HRID 1579376노트

반응식

HRID 1579376 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 12898475HCID 12898475, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0f4bfea9a1524446bb412c55e466c363
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931199

반응 노트

불러오는 중…