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Triethylamine → HCID 71258840, 화합물

HRID 1424830
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HRID 1424830 반응식
CCN(CC)CC.[Br:8][C:9]1[CH:14]=[CH:13][C:12](B(O)O)=[CH:11][C:10]=1[Cl:18].[NH2:19][C:20]1[C:40]([CH:41]2[CH2:43][CH2:42]2)=[CH:39][C:23]2[C:24]([C:34]([O:36][CH2:37][CH3:38])=[O:35])=[C:25]([C:27]3[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=3)[O:26][C:22]=2[CH:21]=1.CCOC(C)=O>C(Cl)Cl.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[Br:8][C:9]1[CH:14]=[CH:13][C:12]([NH:19][C:20]2[C:40]([CH:41]3[CH2:43][CH2:42]3)=[CH:39][C:23]3[C:24]([C:34]([O:36][CH2:37][CH3:38])=[O:35])=[C:25]([C:27]4[CH:28]=[CH:29][C:30]([Cl:33])=[CH:31][CH:32]=4)[O:26][C:22]=3[CH:21]=2)=[CH:11][C:10]=1[Cl:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471Triethylamine4회HCID 8857Ethyl AcetateHCID 46739822(4-Bromo-3-chlorophenyl)boronic acid3회HCID 67354469HCID 67354469, 화합물

생성물 1

HCID 71258840HCID 71258840, 화합물수율 88%

시약·촉매·용매 2

HCID 8895
Cupric acetate
촉매
3회
HCID 6344Dichloromethane용매4회

실험 절차

NEt3 (0.490 mL, 3.51 mmol) was added to a suspension of (4-bromo-3-chlorophenyl)boronic acid (364 mg, 1.546 mmol) in DCM (7 mL) and the resulting solution was added dropwise to mixture of ethyl 6-amino-2-(4-chlorophenyl)-5-cyclopropylbenzofuran-3-carboxylate (500 mg, 1.405 mmol), copper(II) acetate (281 mg, 1.546 mmol), 3 Å molecular sieves (1 g) and NEt3 (0.490 mL, 3.51 mmol) in DCM (7 mL) stirring vigorously at RT open to the air in a flask equipped with a drying tube. After stirring for 4 h at RT, another solution of NEt3 (0.490 mL, 3.51 mmol) and (4-bromo-3-chlorophenyl)boronic acid (364 mg, 1.546 mmol) in DCM (7 mL) was added dropwise to the reaction mixture, followed by more copper(II) acetate (281 mg, 1.546 mmol). The reaction mixture was stirred for 3 d and more solution of NEt3 (0.490 mL, 3.51 mmol) and (4-bromo-3-chlorophenyl)boronic acid (364 mg, 1.546 mmol) in DCM (7 mL) was added dropwise with further addition of copper(II) acetate (281 mg, 1.546 mmol). After 2 h, EtOAc was added followed by Celite. The mixture was stirred for 30 min then filtered through a pad of Celite and the brown solution was concentrated to dryness. EtOAc was added followed by water. The organic layer was separated, washed with water, brine, dried over MgSO4, filtered and concentrated. The crude product was purified on silica gel (hex/EtOAc) to give ethyl 6-((4-bromo-3-chlorophenyl)amino)-2-(4-chlorophenyl)-5-cyclopropylbenzofuran-3-carboxylate (685 mg, 1.231 mmol, 88% yield) as an orange foam. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.17 (s, 1H), 7.98-8.07 (m, 2H), 7.58-7.65 (m, 3H), 7.49-7.56 (m, 2H), 7.11 (d, 1H), 6.87 (dd, 1H), 4.36 (q, 2H), 1.95-2.12 (m, 1H), 1.36 (t, 3H), 0.93-1.05 (m, 2H), 0.57-0.71 (m, 2H).

후처리

  1. customequipped with a drying tube
  2. stirringAfter stirring for 4 h at RT
  3. stirringThe reaction mixture was stirred for 3 d
  4. stirringThe mixture was stirred for 30 min
  5. filtrationthen filtered through a pad of Celite
  6. concentrationthe brown solution was concentrated to dryness
  7. additionEtOAc was added
  8. customThe organic layer was separated
  9. washwashed with water, brine
  10. dry with materialdried over MgSO4
  11. filtrationfiltered
  12. concentrationconcentrated
  13. customThe crude product was purified on silica gel (hex/EtOAc)

출처 및 근거

ORD 기록
ord-cc116782f33942e9b65485691ebb8db6
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08927593B2

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