Hydrochloric Acid → HCID 12274208, 화합물

HRID 1579378노트

반응식

HRID 1579378 반응식
[ClH:1].[N:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[CH2:8][C:9]3[CH:15]=[CH:14][CH:13]=[CH:12][C:10]=3[O:11][C:3]=12.[CH2:16]=O.S(=O)(=O)(O)O.C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:1][CH2:16][C:14]1[CH:13]=[CH:12][C:10]2[O:11][C:3]3=[N:2][CH:7]=[CH:6][CH:5]=[C:4]3[CH2:8][C:9]=2[CH:15]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric Acid2회HCID 712Formaldehyde2회HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 122742075H-chromeno[2,3-b]pyridine

생성물 1

HCID 12274208HCID 12274208, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Hydrogen chloride gas is passed through a mixture of 10 g of 5H-[1]benzopyrano[2,3-b]pyridine, 1.4 g of paraformaldehyde, 110 ml of concentrated sulfuric acid and 22 ml of concentrated hydrochloric acid at 80°C for 12 hours, while 2 g of paraformaldehyde is added in several portions to the reaction mixture. The reaction mixture is poured into water, and the whole mixture is neutralized with sodium carbonate, and extracted with a large amount of chloroform. The chloroform layer is dried, concentrated to 30 ml, and cooled. The crystalline precipitate is filtered off, and recrystallized from chloroform to give 7-chloromethyl-5H-[1]benzopyrano[2,3-b]pyridine melting at 172°-174°C.

후처리

  1. additionis added in several portions to the reaction mixture
  2. extractionextracted with a large amount of chloroform
  3. dry with materialThe chloroform layer is dried
  4. concentrationconcentrated to 30 ml
  5. temperaturecooled
  6. filtrationThe crystalline precipitate is filtered off
  7. customrecrystallized from chloroform

출처 및 근거

ORD 기록
ord-e603d10ad4084d83a811f6875b59cedb
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931199

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