Sodium Hydroxide → Methyl (4-iodo-5-methylpyridin-2-yl)carbamate

HRID 537032ノート

反応式

HRID 537032 の反応式
[CH3:1][O:2][C:3]([N:5]([C:10]1[CH:15]=[C:14]([I:16])[C:13]([CH3:17])=[CH:12][N:11]=1)C(OC)=O)=[O:4].[OH-].[Na+]>CO>[CH3:1][O:2][C:3](=[O:4])[NH:5][C:10]1[CH:15]=[C:14]([I:16])[C:13]([CH3:17])=[CH:12][N:11]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 66748316Dimethyl(4-iodo-5-methylpyridin-2-yl)imidodicarbonate

生成物 1

HCID 67952848Methyl (4-iodo-5-methylpyridin-2-yl)carbamate収率 75.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Dimethyl(4-iodo-5-methylpyridin-2-yl)imidodicarbonate (110 g, 310 mmol) was added to a mixture of MeOH (1500 mL) and 1M NaOH (620 mL). The reaction mixture was allowed to stir at rt for 1.5 h and was then concentrated. EtOAc and water were added to the residue and the solution was extracted with EtOAc. The organic solutions were combined, washed with brine, dried over Na2SO4, filtered and concentrated to give methyl(4-iodo-5-methylpyridin-2-yl)carbamate (68 g, 60%) which was used in the next step without purification.

後処理

  1. concentrationwas then concentrated
  2. additionEtOAc and water were added to the residue
  3. extractionthe solution was extracted with EtOAc
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-8de1e3babf17429e99ca7dcda2c8e749
出典データセット
uspto-grants-2014_10
特許番号
US08859768B2

反応ノート

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