Hydrochloric Acid → HCID 13136928, 화합물

HRID 851200노트

반응식

HRID 851200 반응식
N[C:2]1[C:3]([CH3:17])=[CH:4][C:5]2[O:15][C:14](=[O:16])[C:9]3[CH2:10][NH:11][CH2:12][CH2:13][C:8]=3[C:6]=2[CH:7]=1.N([O-])=O.[Na+].C(=O)([O-])[O-].[K+].[K+].[ClH:28]>O>[Cl:28][C:2]1[C:3]([CH3:17])=[CH:4][C:5]2[O:15][C:14](=[O:16])[C:9]3[CH2:10][NH:11][CH2:12][CH2:13][C:8]=3[C:6]=2[CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 11430Potassium CarbonateHCID 13136926HCID 13136926, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 13136928HCID 13136928, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
-5 °C

실험 절차

Concentrated hydrochloric acid (8 ml) is added to a stirred suspension of 9-amino-1,2,3,4-tetrahydro-8-methyl-5H-[1]benzopyrano[3,4-c]pyridin-5-one (1.5 g, 0.0065 moles) in water (5 ml). The solution is cooled to -5° C. and a solution of sodium nitrite (0.45 g, 0.0065 moles) in water (4 ml) is added dropwise. After 15 minutes the mixture is added to a solution of freshly prepared cuprous chloride (0.8 g, 0.008 moles) in 20% HCl (8 ml) and stirred for 15 minutes. The suspension is warmed on the steam bath for one hour, allowed to cool, and 10% aqueous potassium carbonate is added until the mixture is basic. The precipitate is filtered off, rinsed with water, dissolved in warm dilute hydrochloric acid, filtered, and reprecipitated by the addition of concentrated ammonium hydroxide. The precipiate is filtered off, rinsed with water, and dried. Recrystallization from ethyl acetate gave the product (0.8 g), mp 184°- 185° C.

후처리

  1. temperatureThe suspension is warmed on the steam bath for one hour
  2. temperatureto cool
  3. filtrationThe precipitate is filtered off
  4. washrinsed with water
  5. dissolutiondissolved
  6. temperaturein warm dilute hydrochloric acid
  7. filtrationfiltered
  8. customreprecipitated by the addition of concentrated ammonium hydroxide
  9. filtrationThe precipiate is filtered off
  10. washrinsed with water
  11. customdried
  12. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-80bf8df6347c4f9695dfa6d2923cdb4f
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04382939

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