Morpholine → HCID 59354746、化合物

HRID 655411

反応式

HRID 655411 の反応式
Br[C:2]1[C:3]([N:5]([CH3:10])[C:6](=[O:9])[C:7]=1[Br:8])=[O:4].C([O-])([O-])=O.[Cs+].[Cs+].[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1>CN(C=O)C>[Br:8][C:7]1[C:6](=[O:9])[N:5]([CH3:10])[C:3](=[O:4])[C:2]=1[N:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1

参加物

5

反応物 3

HCID 8083MorpholineHCID 10796Cesium carbonateHCID 181552,3-Dibromo-N-methylmaleimide

生成物 1

HCID 59354746HCID 59354746、化合物収率 85%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a room temperature, stirred solution of 2,3-dibromo-N-methylmaleimide (1 g, 0.004 mol) in DMF (10 mL) was added Cs2CO3 (1.34 g, 0.004 mol) followed by morpholine (360 mg, 0.004 mol) under N2 atmosphere. The reaction mixture was then stirred for 30 minutes, quenched with ice water, and extracted with EtOAc (2×50 mL). The combined organic layers were washed with water, dried over anhydrous Na2SO4, filtered and concentrated in vacuo to afford 3-bromo-1-methyl-4-morpholino-1H-pyrrole-2,5-dione (0.87 g, 85%) as a solid.

後処理

  1. customquenched with ice water
  2. extractionextracted with EtOAc (2×50 mL)
  3. washThe combined organic layers were washed with water
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bd46410cdf5d4ea8a204638e358eb277
出典データセット
uspto-grants-2011_12
特許番号
US08071595B2

関連ノート

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