Sodium Iodide → HCID 46919443, 화합물

HRID 77351

반응식

HRID 77351 반응식
[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9]Cl)=[O:7])=[CH:4][CH:3]=1.[Na+].[I-:14]>CC(C)=O>[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][I:14])=[O:7])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 11401232Chloromethyl 4-fluorobenzoate

생성물 1

HCID 46919443HCID 46919443, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a solution of chloromethyl 4-fluorobenzoate (3.0g, 15.9 mmol) in 50 mL of dry acetone, NaI (4.8 g, 31.8 mmol) was added and the mixture was stirred overnight. The solvent was removed and Et2O (150 mL) was added to the solid residues and the mixture was stirred for 10 min. After filtration the filtrate was washed with 5% NaHSO3 (aq) (2×25 mL) followed by brine. The organic solution was concentrated by rotary evaporation and purified by silica gel chromatography to give a light yellow oil. Yield 3.7 g (85%). 1H NMR (300 MHz, CDCl3): δ 6.16 (s, 2H), 7.17 (m, 2H), 8.08 (m, 2H).

후처리

  1. customThe solvent was removed
  2. additionEt2O (150 mL) was added to the solid residues
  3. stirringthe mixture was stirred for 10 min
  4. filtrationAfter filtration the filtrate
  5. washwas washed with 5% NaHSO3 (aq) (2×25 mL)
  6. concentrationThe organic solution was concentrated by rotary evaporation
  7. custompurified by silica gel chromatography
  8. customto give a light yellow oil

출처 및 근거

ORD 기록
ord-3a7da02939a042cb873473416ffb7bfe
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841257B2

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