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

HRID 457695ノート

反応式

HRID 457695 の反応式
[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

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 11471166HCID 11471166、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de809e1a6f4f49b19078eba5b834587e
出典データセット
uspto-grants-2007_03
特許番号
US07189730B2

反応ノート

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