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N-Iodosuccinimide → (4-Iodo-3-methylisoxazol-5-yl)acetic acid methyl ester

HRID 922243
ノート
印刷プレビュー

反応式

HRID 922243 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([CH2:7][C:8]([O:10][CH3:11])=[O:9])[O:4][N:3]=1.[I:12]N1C(=O)CCC1=O>FC(F)(F)C(O)=O>[I:12][C:6]1[C:2]([CH3:1])=[N:3][O:4][C:5]=1[CH2:7][C:8]([O:10][CH3:11])=[O:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 12366875Methyl 2-(3-methylisoxazol-5-yl)acetate

生成物 1

HCID 66685715(4-Iodo-3-methylisoxazol-5-yl)acetic acid methyl ester収率 72.4%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

反応条件

温度
65 °C

実験手順

To a sealed tube fitted with magnetic stirrer was charged methyl (3-methyl-1,2-oxazol-5-yl)acetate (0.9 g, 5.8 mmol) and N-iodosuccinimide (2.61 g, 11.6 mmol) in 10 mL trifluoroacetic acid. The reaction mixture was heated at 65° C. for 3 h. The RM was quenched with NaHCO3 solution (25 mL) and extracted with ethyl acetate (30 mL). The organic layer was washed with water (30 mL) and saturated brine solution (30 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as brown solid (1.18 g, yield: 72.4%).

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  1. customTo a sealed tube fitted with magnetic stirrer
  2. customThe RM was quenched with NaHCO3 solution (25 mL)
  3. extractionextracted with ethyl acetate (30 mL)
  4. washThe organic layer was washed with water (30 mL) and saturated brine solution (30 mL)
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-b802d6b9b7f54f6ba2613b59b6818ddd
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278915B2

反応ノート

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