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

HRID 390248노트

반응식

HRID 390248 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b5fe6826cde04b8492bcb612a7d34384
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383637B2

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