Hydrochloric Acid → HCID 20509910、化合物

HRID 1758235ノート

反応式

HRID 1758235 の反応式
COC(OC)CNCC1C=C(C)C=CC=1N.N#CBr.[NH2:20][C:21]1[N:30]([CH2:31][CH:32](OC)OC)[CH2:29][C:28]2[C:23](=[CH:24][CH:25]=[C:26]([CH3:37])[CH:27]=2)[N:22]=1.Cl>C(O)C>[CH3:37][C:26]1[CH:27]=[C:28]2[C:23](=[CH:24][CH:25]=1)[NH:22][C:21]1=[N:20][CH:32]=[CH:31][N:30]1[CH2:29]2

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10476Cyanogen BromideHCID 20509899HCID 20509899、化合物HCID 20509920HCID 20509920、化合物

生成物 1

HCID 20509910HCID 20509910、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

45 g of N-(2-amino-5-methylbenzyl)-aminoacetaldehydedimethylacetal obtained in step (d) and 25 g of cyanogen bromide are heated under reflux in 500 ml of 95% ethanol for 18 hours. After the mixture containing 2-amino-3-(2,2-dimethoxyethyl)-6-methyl-3,4-dihydroquinazoline is cooled, 200 ml of 5 N hydrochloric acid are added, and the solution is left to stand for 2 hours at room temperature. After the reaction solution is concentrated in a vacuum, it is made alkaline with dilute caustic soda, whereupon the title compound crystallizes out, and is recrystallised from methanol or ethanol. M.p. 265° C.

後処理

  1. temperatureis cooled
  2. waitthe solution is left
  3. concentrationAfter the reaction solution is concentrated in a vacuum, it
  4. customwhereupon the title compound crystallizes out, and
  5. customis recrystallised from methanol or ethanol

出典と根拠

ORDレコード
ord-cff7473dd8184b4fa574fa6adafe38ac
出典データセット
uspto-grants-1983_02
特許番号
US04372956

反応ノート

読み込み中…