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Triethylamine → Methyl 2-chloro-3-[4-(2-(4-[(methylsulfonyl)oxy]phenoxy)ethyl)phenyl]propanoate

HRID 1178566
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HRID 1178566 반응식
[Cl:1][CH:2]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)=[CH:10][CH:9]=1)[C:3]([O:5][CH3:6])=[O:4].C(N(CC)CC)C.[CH3:31][S:32](Cl)(=[O:34])=[O:33]>ClCCl>[Cl:1][CH:2]([CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][O:16][C:17]2[CH:18]=[CH:19][C:20]([O:23][S:32]([CH3:31])(=[O:34])=[O:33])=[CH:21][CH:22]=2)=[CH:10][CH:9]=1)[C:3]([O:5][CH3:6])=[O:4]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 86600804Methyl 2-chloro-3-(4-[2-(4-hydroxyphenoxy)ethyl]phenyl)propanoate

생성물 1

HCID 11407297Methyl 2-chloro-3-[4-(2-(4-[(methylsulfonyl)oxy]phenoxy)ethyl)phenyl]propanoate수율 96%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
-20 °C

실험 절차

Methyl 2-chloro-3-{4-[2-(4-hydroxyphenoxy)ethyl]phenyl}propanoate (334 mg, 1.0 mmol) and triethylamine (303 mg, 3.0 mmol) was dissolved in 20 ml dichlormethane and cooled to −20° C. under nitrogen atmosphere. Methanesulfonyl chloride (114 mg, 1.0 mmol) was added dropwise. The mixture was allowed to reach room temperature. After 2 hours dichlormethane was added, the mixture was washed (water, brine), dried (Na2SO4) and evaporated under reduced pressure to yield 394 mg pure product (yield 96%).

후처리

  1. customto reach room temperature
  2. washthe mixture was washed (water, brine)
  3. dry with materialdried (Na2SO4)
  4. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-da0989c48a814faba11ce697e5554013
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07276539B2

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