Triethylamine → Methyl 2-{[4-(3-{4-[(methylsulfonyl)oxy]phenoxy}propyl)phenoxy]methyl}benzoate

HRID 2112022노트

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HRID 2112022 반응식
[OH:1][C:2]1[CH:29]=[CH:28][C:5]([O:6][CH2:7][CH2:8][CH2:9][C:10]2[CH:27]=[CH:26][C:13]([O:14][CH2:15][C:16]3[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=3[C:18]([O:20][CH3:21])=[O:19])=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH3:37][S:38](Cl)(=[O:40])=[O:39]>ClCCl>[CH3:37][S:38]([O:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][CH2:8][CH2:9][C:10]2[CH:27]=[CH:26][C:13]([O:14][CH2:15][C:16]3[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=3[C:18]([O:20][CH3:21])=[O:19])=[CH:12][CH:11]=2)=[CH:28][CH:29]=1)(=[O:40])=[O:39]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 68869776Methyl 2-({4-[3-(4-hydroxyphenoxy)propyl]phenoxy}methyl)benzoate

생성물 1

HCID 86601926Methyl 2-{[4-(3-{4-[(methylsulfonyl)oxy]phenoxy}propyl)phenoxy]methyl}benzoate수율 97.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
-20 °C

실험 절차

Methyl 2-({4-[3-(4-hydroxyphenoxy)propyl]phenoxy}methyl)benzoate (0.32 g, 0.81 mmol) was dissolved in dichloromethane (10 ml) and cooled to −20° C. Triethylamine (0.123 g, 1.22 mmol) was added drop wise and methanesulfonyl chloride (0.10 g, 0.89 mmol) was added drop wise. The ice bath was removed and the mixture was wormed to room temperature. Diethyl ether (5 ml) was added and the precipitate was filtered off. The organic phase was washed with two portions of brine (5 ml) and dried (MgSO4). Removing the solvent by evaporation gave 0.37 gram of methyl 2-{[4-(3-{4-[(methylsulfonyl)oxy]-phenoxy}propyl)phenoxy]methyl}benzoate (yield 97.3%).

후처리

  1. customThe ice bath was removed
  2. customwas wormed to room temperature
  3. additionDiethyl ether (5 ml) was added
  4. filtrationthe precipitate was filtered off
  5. washThe organic phase was washed with two portions of brine (5 ml)
  6. dry with materialdried (MgSO4)
  7. customRemoving the solvent
  8. customby evaporation

출처 및 근거

ORD 기록
ord-1a00703168db48169f1028b26374011d
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07521461B2

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