N-bromobutanimide → HCID 67142870、化合物

HRID 1245553ノート

反応式

HRID 1245553 の反応式
[C:1]([NH:4][C:5]1[C:6]2[CH:13]=[CH:12][N:11]([C@@H:14]3[O:26][C@H:25]([CH2:27][O:28][C:29](=[O:31])[CH3:30])[C@@H:20]([O:21][C:22](=[O:24])[CH3:23])[C@@:15]3([CH3:32])[O:16][C:17](=[O:19])[CH3:18])[C:7]=2[N:8]=[CH:9][N:10]=1)(=[O:3])[CH3:2].[Br:33]N1C(=O)CCC1=O>CN(C=O)C>[C:1]([NH:4][C:5]1[C:6]2[C:13]([Br:33])=[CH:12][N:11]([C@@H:14]3[O:26][C@H:25]([CH2:27][O:28][C:29](=[O:31])[CH3:30])[C@@H:20]([O:21][C:22](=[O:24])[CH3:23])[C@@:15]3([CH3:32])[O:16][C:17](=[O:19])[CH3:18])[C:7]=2[N:8]=[CH:9][N:10]=1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 67142229HCID 67142229、化合物

生成物 1

HCID 67142870HCID 67142870、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
0 °C

実験手順

To a pre-cooled (0° C.) solution of the compound from Step A (460 mg, 1.00 mmol) in DMF is added N-bromosuccinimide (178 mg, 1.0 mmol) in DMF. The resulting solution is stirred at 0° C. for 30 min then at room temperature for another 30 min. The reaction is quenched by addition of methanol and evaporated in vacuo. The resulting crude mixture is purified on silica gel using ethyl acetate/hexane as the eluent. Fractions containing the desired product are pooled and evaporated in vacuo to give the desired product.

後処理

  1. waitat room temperature for another 30 min
  2. customThe reaction is quenched by addition of methanol
  3. customevaporated in vacuo
  4. customThe resulting crude mixture is purified on silica gel
  5. additionFractions containing the desired product
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-5a2151723b5a45999e4bd92a9a887311
出典データセット
uspto-grants-2006_10
特許番号
US07125855B2

反応ノート

読み込み中…