Acetic Acid → HCID 13229174, 화합물

HRID 1579379노트

반응식

HRID 1579379 반응식
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

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 12274208HCID 12274208, 화합물

생성물 1

HCID 13229174HCID 13229174, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

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 dioxane

출처 및 근거

ORD 기록
ord-b2b560df89df427fb3318e78da2a6ef1
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931199

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