Hydrochloric Acid → HCID 136005323、化合物

HRID 2052281ノート

反応式

HRID 2052281 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([CH3:15])=[N:13][N:14]=[C:7]1[N:6]=[C:5]2[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[BH4-].[Na+].Cl>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([CH3:15])=[N:13][N:14]=[C:7]1[NH:6][CH:5]2[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 1869146[1,2,4]Triazolo[4,3-a]quinazoline, 7-chloro-1-methyl-5-phenyl-HCID 4311764Sodium borohydride

生成物 1

HCID 136005323HCID 136005323、化合物収率 57.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 1.3 g of 7-chloro-1-methyl-5-phenyl-s-triazolo[4,3-a]quinazoline in 70 ml of dimethylformamide was added 0.5 g of sodium borohydride. The mixture was heated with stirring at 75°-80° C. for 2 hours and then poured into ice-water. The resulting mixture was neutralized with dilute hydrochloric acid, and the precipitate formed was collected by filtration and washed with water. The solid was then suspended in a mixture of 40 ml of methanol and 5 ml of concentrated hydrochloric acid, and the mixture was stirred at room temperature for 2 hours. After neutralization with ammonia water, the mixture was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. The residue was recrystallized from dimethylformamideethanol to give 0.75 g of 7-chloro-4,5-dihydro-1-methyl-5-phenyl-s-triazolo[4,3-a]quinazoline as colorless needles, m.p. 262°-265° C.

後処理

  1. temperatureThe mixture was heated
  2. customthe precipitate formed
  3. filtrationwas collected by filtration
  4. washwashed with water
  5. additionThe solid was then suspended in a mixture of 40 ml of methanol and 5 ml of concentrated hydrochloric acid
  6. stirringthe mixture was stirred at room temperature for 2 hours
  7. extractionAfter neutralization with ammonia water, the mixture was extracted with chloroform
  8. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
  9. customthe solvent was removed under reduced pressure
  10. customThe residue was recrystallized from dimethylformamideethanol

出典と根拠

ORDレコード
ord-7d1b58d5e5dd49e9b91ac0b77b7c893f
出典データセット
uspto-grants-1980_01
特許番号
US04183932

反応ノート

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