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Water → Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate

HRID 385030
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HRID 385030 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1[OH:15])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:3])[CH3:2].[I:16]N1C(=O)CCC1=O.FC(F)(F)S(O)(=O)=O.O>ClCCl.CO>[C:1]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([I:16])[C:14]=1[OH:15])[C:8]([O:10][CH3:11])=[O:9])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

7

반응물 4

HCID 962WaterHCID 62406Trifluoromethanesulfonic acidHCID 120273N-IodosuccinimideHCID 13207060Methyl 3-tert-butyl-4-hydroxybenzoate

생성물 1

HCID 12084815Methyl 3-t-butyl-4-hydroxy-5-iodobenzoate수율 94.3%

시약·촉매·용매 2

HCID 887Methanol
용매
HCID 6344Dichloromethane용매

실험 절차

Methyl 3-t-butyl-4-hydroxybenzoate (1.83 g) was dissolved in dichloromethane (24 mL) and methanol (3 mL), and N-iodosuccinimide (2.08 g) and trifluoromethanesulfonic acid (3 mL) were added to the solution, and then the mixture was stirred at room temperature for 15 minutes. Water was added to the reaction solution, and then the organic layer was separated. The organic layer was washed with 10% sodium thiosulfate and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (2.77 g) as a brown crystal.

후처리

  1. customthe organic layer was separated
  2. washThe organic layer was washed with 10% sodium thiosulfate and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-5c22d3a8a061459990ebdc6a40e1ca1c
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367843B2

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