Methyl iodide → Tert-butyl 2-methyl-1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate

HRID 1036732ノート

反応式

HRID 1036732 の反応式
[O:1]=[C:2]1[C:5]2([CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:6]2)[CH:4]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[NH:3]1.[H-].[Na+].I[CH3:27]>CN(C=O)C>[CH3:27][N:3]1[CH:4]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[C:5]2([CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:6]2)[C:2]1=[O:1]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 71060527rac-tert-Butyl 1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate

生成物 1

HCID 71060344Tert-butyl 2-methyl-1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A stirred solution of rac-tert-butyl 1-oxo-3-phenyl-2,6-diazaspiro[3.5]nonane-6-carboxylate (1.18 g, 3.73 mmol) in DMF (20 ml) was cooled to 0° C. and treated with NaH (194 mg, 4.85 mmol) followed by iodomethane (303 ul, 4.85 mmol). The mixture was left to warm to room temperature. After 5 hours, the reaction was quenched with water and extracted with ethyl acetate. The organic layer was separated and washed with brine, dried (MgSO4) and concentrated in vacuo to yield a the title compound as a yellow oil;

後処理

  1. waitThe mixture was left
  2. customthe reaction was quenched with water
  3. extractionextracted with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-716b629e2a844ffda196e1267644840c
出典データセット
uspto-grants-2013_10
特許番号
US08546416B2

反応ノート

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