Cyanogen Bromide → 3-(2-Amino-6-benzoylquinazolin-3(4H)-YL)-N-cyclohexyl-N-methylpropanamide

HRID 390248ノート

反応式

HRID 390248 の反応式
[N:1]#[C:2]Br.[NH2:4][C:5]1[CH:24]=[CH:23][C:22]([C:25](=[O:32])[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:21][C:6]=1[CH2:7][NH:8][CH2:9][CH2:10][C:11]([N:13]([CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[CH3:14])=[O:12]>CO>[NH2:1][C:2]1[N:8]([CH2:9][CH2:10][C:11]([N:13]([CH:15]2[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]2)[CH3:14])=[O:12])[CH2:7][C:6]2[C:5](=[CH:24][CH:23]=[C:22]([C:25](=[O:32])[C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH:21]=2)[N:4]=1

参加物

4

反応物 2

HCID 10476Cyanogen BromideHCID 586251113-(2-Amino-5-benzoyl-benzylamino)-N-cyclohexyl-N-methyl-propionamide

生成物 1

HCID 167412383-(2-Amino-6-benzoylquinazolin-3(4H)-YL)-N-cyclohexyl-N-methylpropanamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Cyanogen bromide (0.011 mol) was added to a solution of 3-(2-amino-5-benzoyl-benzylamino)-N-cyclohexyl-N-methyl-propionamide (0.01 mol) in methanol (200 mL), stirred at room temperature. The reaction solution was stirred over a weekend at room temperature, then stirred and refluxed for an additional 5 h. The solvent was evaporated to yield a residue. The residue was crystallized from ethyl acetate (100 mLI). The resulting precipitate was filtered off and dried. The product fraction was recrystallized from 2-propanol (50 mL). The crystals were filtered off and dried to yield the title compound as a residue.

後処理

  1. stirringThe reaction solution was stirred over a weekend at room temperature
  2. stirringstirred
  3. temperaturerefluxed for an additional 5 h
  4. customThe solvent was evaporated
  5. customto yield a residue
  6. customThe residue was crystallized from ethyl acetate (100 mLI)
  7. filtrationThe resulting precipitate was filtered off
  8. customdried
  9. customThe product fraction was recrystallized from 2-propanol (50 mL)
  10. filtrationThe crystals were filtered off
  11. customdried

出典と根拠

ORDレコード
ord-b5fe6826cde04b8492bcb612a7d34384
出典データセット
uspto-grants-2013_02
特許番号
US08383637B2

反応ノート

読み込み中…