Methyl iodide → 7-Bromo-2-(methylthio)benzo[d]oxazole

HRID 469822ノート

反応式

HRID 469822 の反応式
[Br:1][C:2]1[C:10]2[O:9][C:8]([SH:11])=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[C:12]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C>[Br:1][C:2]1[C:10]2[O:9][C:8]([S:11][CH3:12])=[N:7][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 178527769HCID 178527769、化合物

生成物 1

HCID 674568117-Bromo-2-(methylthio)benzo[d]oxazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 6 g (26.1 mmol) 7-bromo-benzooxazole-2-thiol, 7.28 g (52.2 mmol) K2CO3, 4.1 g (28.7 mmol) MeI in 80 ml DMF is stirred at room temperature for 1 h. The reaction mixture is then poured on water and extracted 2× with EtOAc. The combined organic layers are washed with water and saturated NaCl solution, dried over MgSO4, filtered and the filtrate is concentrated in vacuo to afford the title compound.

後処理

  1. additionThe reaction mixture is then poured on water
  2. extractionextracted 2× with EtOAc
  3. washThe combined organic layers are washed with water and saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-c25e223ba1c24721a93ba704c882b175
出典データセット
uspto-grants-2014_01
特許番号
US08629168B2

反応ノート

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