N-bromobutanimide → 2-benzylamino-8-bromo-9-ethyl-9H-purin-6-ylamine

HRID 457695노트

반응식

HRID 457695 반응식
[CH2:1]([NH:8][C:9]1[N:17]=[C:16]2[C:12]([N:13]=[CH:14][N:15]2[CH2:18][CH3:19])=[C:11]([NH2:20])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:21]N1C(=O)CCC1=O>CN(C=O)C>[CH2:1]([NH:8][C:9]1[N:17]=[C:16]2[C:12]([N:13]=[C:14]([Br:21])[N:15]2[CH2:18][CH3:19])=[C:11]([NH2:20])[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 11471166HCID 11471166, 화합물

생성물 1

HCID 98630752-benzylamino-8-bromo-9-ethyl-9H-purin-6-ylamine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-benzylamino-9-ethyl-9H-purin-6-ylamine (1.0 mmol), a compound of formula (4), in 10 mL of dry DMF was added N-bromosuccinimide (267 mg, 1.5 mmol). The reaction mixture was stirred at room temperature for 1 hour. The solvent was then removed in vacuo and the residue partitioned between water and chloroform. The organic layer was washed with 1N sodium hydroxide, dried (Na2SO4), filtered, and the filtrate concentrated in vacuo. The residue was chromatographed on a silica gel column, eluting with chloroform/methanol; (98/2), to give 2-benzylamino-8-bromo-9-ethyl-9H-purin-6-ylamine as a chromatographically pure solid.

후처리

  1. customThe solvent was then removed in vacuo
  2. customthe residue partitioned between water and chloroform
  3. washThe organic layer was washed with 1N sodium hydroxide
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated in vacuo
  7. customThe residue was chromatographed on a silica gel column
  8. washeluting with chloroform/methanol

출처 및 근거

ORD 기록
ord-de809e1a6f4f49b19078eba5b834587e
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07189730B2

반응 노트

불러오는 중…