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

HRID 922243
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HRID 922243 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

반응 조건

온도
65 °C

실험 절차

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%).

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  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

출처 및 근거

ORD 기록
ord-b802d6b9b7f54f6ba2613b59b6818ddd
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278915B2

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