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Triethylamine → 3-Morpholin-4-ylphenyl trifluoromethanesulfonate

HRID 2179575
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반응식

HRID 2179575 반응식
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].[N:16]1([C:22]2[CH:23]=[C:24](O)[CH:25]=[CH:26][CH:27]=2)[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.C(N(CC)CC)C>ClCCl>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:26]1[CH:25]=[CH:24][CH:23]=[C:22]([N:16]2[CH2:17][CH2:18][O:19][CH2:20][CH2:21]2)[CH:27]=1)(=[O:5])=[O:4]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 67749Trifluoromethanesulfonic anhydrideHCID 1413433-Morpholinophenol

생성물 1

HCID 179826773-Morpholin-4-ylphenyl trifluoromethanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-10 °C

실험 절차

2.18 ml (12.9 mmol) of trifluoromethanesulphonic anhydride are slowly added dropwise to a solution, cooled to −10° C., of 1.54 g (8.6 mmol) of 3-(4-morpholinyl)-phenol and 3.59 ml (25.8 mmol) of triethylamine in 10 ml of dichloromethane. The mixture is stirred at −10° C. for 30 min and then at 0° C. for 30 min. It is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution, dried over sodium sulphate and concentrated in vacuo, and the residue is dried under high vacuum. 2.41 g (90.1% of theory) of the title compound are obtained.

후처리

  1. waitat 0° C. for 30 min
  2. washIt is washed successively with 10% strength sodium bicarbonate solution, water and saturated sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue is dried under high vacuum

출처 및 근거

ORD 기록
ord-a463712e7d664db08f3b179ce23cee64
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09067931B2

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