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Cesium carbonate → Tert-butyl 2-[4-[4-(trifluoromethylsulfonyl)anilino]cyclohexoxy]acetate

HRID 1772290
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HRID 1772290 반응식
[NH2:1][CH:2]1[CH2:7][CH2:6][CH:5]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:4][CH2:3]1.Br[C:18]1[CH:23]=[CH:22][C:21]([S:24]([C:27]([F:30])([F:29])[F:28])(=[O:26])=[O:25])=[CH:20][CH:19]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C1(C)C=CC=CC=1.CC([O-])=O.CC([O-])=O.[Pd+2].C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1>[F:29][C:27]([F:28])([F:30])[S:24]([C:21]1[CH:22]=[CH:23][C:18]([NH:1][CH:2]2[CH2:7][CH2:6][CH:5]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:4][CH2:3]2)=[CH:19][CH:20]=1)(=[O:25])=[O:26]
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참가 물질

7

반응물 3

HCID 10796Cesium carbonateHCID 3001141-Bromo-4-trifluoromethanesulfonylbenzeneHCID 10680931Tert-butyl 2-(4-aminocyclohexoxy)acetate

생성물 1

HCID 86719526Tert-butyl 2-[4-[4-(trifluoromethylsulfonyl)anilino]cyclohexoxy]acetate수율 98.2%

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매
HCID 634876
Binap, (A+-)-
촉매
HCID 1140Toluene용매

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온도
100 °C

실험 절차

A suspension of tert-butyl 2-(4-aminocyclohexoxy)acetate (0.5 g, 1.7 mmol, 1 eq.), 1-bromo-4-(trifluoromethylsulfonyl)benzene (0.4 g, 1.7 mmol, 1 eq.), cesium carbonate (1.4 g, 4.3 mmol, 2.5 eq.), and BINAP (54 mg, 0.08 mmol, 0.05 eq.), in toluene (15 mL), was bubbled with nitrogen for 10 minutes before the addition of Pd(OAc)2 (19 mg, 0.08 mmol, 0.05 eq.) to the reaction mixture. Nitrogen gas was bubbled through the reaction mixture for another 10 minutes and the contents were heated at 100° C. under nitrogen atmosphere for 3 hours. The contents were cooled to room temperature, diluted with ethyl acetate, filtered through Celite®, and concentrated. The crude material was purified by silica gel column chromatography using ethyl acetate/heptanes to elute. The product containing fractions were combined and concentrated to obtain tert-butyl 2-[4-[4-(trifluoromethylsulfonyl)anilino]cyclohexoxy]acetate (0.73 g, 77%); (CI, m/z): [M+H]+ 438; 1H NMR (400 MHz, CDCl3): δ 7.74 (d, J=8.9 Hz, 2H), 6.56-6.70 (m, 2H), 4.44 (d, J=7.4 Hz, 1H), 4.02 (s, 2H), 3.32-3.49 (m, 2H), 2.07-2.25 (m, 4H), 1.44-1.55 (m, 11H), 1.21-1.35 (m, 2H).

후처리

  1. customNitrogen gas was bubbled through the reaction mixture for another 10 minutes
  2. temperatureThe contents were cooled to room temperature
  3. additiondiluted with ethyl acetate
  4. filtrationfiltered through Celite®
  5. concentrationconcentrated
  6. customThe crude material was purified by silica gel column chromatography
  7. washto elute
  8. additionThe product containing fractions
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-20714f17df9d4fc2a4b2a7d3457beb87
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249102B2

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