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Triethylamine → 4-(4-Bromo-2,6-difluoro-benzyl)-thiomorpholine 1,1-dioxide

HRID 469828
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반응식

HRID 469828 반응식
[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9]Br)=[C:6]([F:8])[CH:7]=1.[CH2:12]1[NH:19][CH2:18][CH2:17][S:14](=[O:16])(=[O:15])[CH2:13]1.C(N(CC)CC)C>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([F:11])[C:5]([CH2:9][N:19]2[CH2:18][CH2:17][S:14](=[O:16])(=[O:15])[CH2:13][CH2:12]2)=[C:6]([F:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27733055-Bromo-2-(bromomethyl)-1,3-difluorobenzeneHCID 6484228Thiomorpholine 1,1-dioxide

생성물 1

HCID 674580134-(4-Bromo-2,6-difluoro-benzyl)-thiomorpholine 1,1-dioxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 3.8 g (11.3 mmol) 5-bromo-2-bromomethyl-1,3-difluoro-benzene, 1.83 g (13.6 mmol) thiomorpholine dioxide and 1.88 ml (13.6 mmol) triethylamine in 40 ml dichloromethane is stirred at room temperature for 20 h. Then the reaction mixture is poured on water and extracted 3× with EtOAc. The combined organic layers are washed with water and saturated NaCl solution, dried over MgSO4, filtered and the filtrate is concentrated in vacuo. The residue is taken up in diethylether, vigorously stirred, and the title compound is obtained after filtration as a white crystalline solid.

후처리

  1. additionThen the reaction mixture is poured on water
  2. extractionextracted 3× with EtOAc
  3. washThe combined organic layers are washed with water and saturated NaCl solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate is concentrated in vacuo

출처 및 근거

ORD 기록
ord-eeeb12cd11ea48a2a44891fb56c1c5eb
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08629168B2

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