tert-Butoxy bis(dimethylamino)methane → 1,1-Dimethylethyl [2-[3-(dimethylamino)-2-fluoroacryloyl]-5-fluoro-6-(methyloxy)-3-pyridinyl]carbamate

HRID 15132

反応式

HRID 15132 の反応式
[F:1][C:2]1[CH:3]=[C:4]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[C:5]([C:10](=[O:13])[CH2:11][F:12])=[N:6][C:7]=1[O:8][CH3:9].[CH3:22][N:23]([CH:25](N(C)C)OC(C)(C)C)[CH3:24]>C1(C)C=CC=CC=1>[CH3:22][N:23]([CH3:25])[CH:24]=[C:11]([F:12])[C:10]([C:5]1[C:4]([NH:14][C:15](=[O:21])[O:16][C:17]([CH3:18])([CH3:20])[CH3:19])=[CH:3][C:2]([F:1])=[C:7]([O:8][CH3:9])[N:6]=1)=[O:13]

参加物

4

反応物 2

HCID 79885tert-Butoxy bis(dimethylamino)methaneHCID 866141471,1-Dimethylethyl [5-fluoro-2-(fluoroacetyl)-6-(methyloxy)-3-pyridinyl]carbamate

生成物 1

HCID 686534721,1-Dimethylethyl [2-[3-(dimethylamino)-2-fluoroacryloyl]-5-fluoro-6-(methyloxy)-3-pyridinyl]carbamate収率 49%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
40 °C

実験手順

A solution of 1,1-dimethylethyl [5-fluoro-2-(fluoroacetyl)-6-(methyloxy)-3-pyridinyl]carbamate (3.72 g, 12.32 mmol) in dry toluene (20 ml) was treated with {(dimethylamino)[(1,1-dimethylethyl)oxy]methyl}dimethylamine (Bredereck's reagent) (3.05 ml, 14.78 mmol) and heated at 40° C. for 2 hours. The mixture was evaporated and the residue triturated with 3×200 ml hexane and the remaining solid dried in vacuo to afford the product (2.15 g, 49%).

後処理

  1. customThe mixture was evaporated
  2. customthe residue triturated with 3×200 ml hexane
  3. customthe remaining solid dried in vacuo

出典と根拠

ORDレコード
ord-087edd2ce0ff4baa9e4675e2e81deb28
出典データセット
uspto-grants-2010_06
特許番号
US07732460B2

関連ノート

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