Hydrochloric Acid → HCID 13136928、化合物

HRID 851200ノート

反応式

HRID 851200 の反応式
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

参加物

6

反応物 4

HCID 313Hydrochloric Acid2 回HCID 11430Potassium CarbonateHCID 13136926HCID 13136926、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 13136928HCID 13136928、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
-5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-80bf8df6347c4f9695dfa6d2923cdb4f
出典データセット
uspto-grants-1983_05
特許番号
US04382939

反応ノート

読み込み中…