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Sodium Carbonate → HCID 59595873, 화합물

HRID 2075146
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HRID 2075146 반응식
[CH2:1]([C:8]1[CH:9]=[CH:10][C:11]2[O:15][C:14](B(O)O)=[CH:13][C:12]=2[CH:19]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][CH:30]=1)[CH2:27][N:26](C(=O)C(F)(F)F)[CH2:25][CH2:24]2.BrC1C=CC=C2C=1CN(C(=O)C(F)(F)F)CC2.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1(C)C=CC=CC=1>[CH2:1]([C:8]1[CH:9]=[CH:10][C:11]2[O:15][C:14]([C:21]3[CH:22]=[C:23]4[C:28](=[CH:29][CH:30]=3)[CH2:27][NH:26][CH2:25][CH2:24]4)=[CH:13][C:12]=2[CH:19]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 231554111-(6-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-2,2,2-trifluoroethanoneHCID 594631661-(8-Bromo-3,4-dihydroisoquinolin-2(1H)-yl)-2,2,2-trifluoroethanoneHCID 59595866(5-Benzylbenzofuran-2-yl)boronic acid

생성물 1

HCID 59595873HCID 59595873, 화합물수율 56%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 702Ethanol용매
HCID 1140Toluene용매

실험 절차

A solution of 5-benzylbenzofuran-2-ylboronic acid (252 mg, 1.0 mmole) in ethanol (3 mL) was added to a mixture of 1-(6-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-2,2,2-trifluoroethanone and 1-(8-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-2,2,2-trifluoroethanone (308 mg, 1.0 mmole), Pd(PPh3)4, toluene, and 2 M Na2CO3(3.5 mL). The resulting mixture was heated at reflux overnight. The reaction was concentrated in vacuo, and the residue was diluted with water. The aqueous phase was extracted with EtOAc (3×50 mL). The combined organic phases were washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified on ISCO column (5% to 10% MeOH/CH2Cl2) to provide the title compounds (189 mg, 56%). 1H NMR (400 MHz, CDCl3) δ 7.60 (m, 2H), 7.39 (dd, 1H), 7.37 (s, 1H), 7.25 (m, 5H), 7.10 (dd, 2H), 6.90 (s, 1H), 4.10 (s, 2H), 3.40 (s, 2H), 3.18 (m, 2H), 2.94 (m, 2H). MS (ESI) m/z: Calculated: 339.16; Observed: 340.10 (M++1).

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. concentrationThe reaction was concentrated in vacuo
  4. additionthe residue was diluted with water
  5. extractionThe aqueous phase was extracted with EtOAc (3×50 mL)
  6. washThe combined organic phases were washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified on ISCO column (5% to 10% MeOH/CH2Cl2)

출처 및 근거

ORD 기록
ord-4819b9989f6d4f1f93c186a0ff393ce6
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919519B2

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