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Triethylamine → Ethyl 2-(2-chloro-4-(3-(3-(tetrahydrofuran-3-yloxy)phenyl)ureido)phenyl)acetate

HRID 1023861
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HRID 1023861 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[C:4]([Cl:14])[CH:3]=1.C(N(CC)CC)C.Cl[C:23](Cl)([O:25]C(=O)OC(Cl)(Cl)Cl)Cl.[O:34]1[CH2:38][CH2:37][CH:36]([O:39][C:40]2[CH:41]=[C:42]([CH:44]=[CH:45][CH:46]=2)[NH2:43])[CH2:35]1>ClCCl>[Cl:14][C:4]1[CH:3]=[C:2]([NH:1][C:23]([NH:43][C:42]2[CH:44]=[CH:45][CH:46]=[C:40]([O:39][CH:36]3[CH2:37][CH2:38][O:34][CH2:35]3)[CH:41]=2)=[O:25])[CH:7]=[CH:6][C:5]=1[CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10]
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 59419389Ethyl 2-(4-amino-2-chlorophenyl)acetateHCID 635571313-(Tetrahydrofuran-3-yloxy)aniline

생성물 1

HCID 67206006Ethyl 2-(2-chloro-4-(3-(3-(tetrahydrofuran-3-yloxy)phenyl)ureido)phenyl)acetate수율 47.1%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
3회

실험 절차

To a solution of ethyl 2-(4-amino-2-chlorophenyl)acetate (240 mg, 1.12 mmol) in dry dichloromethane (4 mL), was added triethylamine (3.13 mL, 22.47 mmol) followed by triphosgene (333 mg, 1.12 mmol) solution in dichloromethane (1 mL). The reaction mixture was stirred at room temperature for 1 h. To this mixture was then added 3-(tetrahydrofuran-3-yloxy)aniline (403 mg, 2.25 mmol) in dichloromethane (1 mL). The reaction mixture was stirred at room temperature for 4 h and concentrated. The residue was dissolved in ethyl acetate and washed with water (2×20 mL), brine (10 mL), dried and concentrated. The crude product was purified by flash column chromatography to afford the desired product as a clear oil (221 mg, 0.528 mmol, 47%). 1H NMR: 1.30 (t, 3H, J=7.2 Hz), 2.05-2.15 (m, 2H), 3.68 (s, 2H), 3.81-3.97 (m, 4H), 4.21 (q, 2H, J=7.2 Hz), 4.82 (d, 1H, J=1.6 Hz), 6.49 (dd, 1H, J=8 Hz, 1.6 Hz), 6.71 (d, 1H, J=7.6 Hz), 7.02-7.11 (m, 4H), 7.18 (s, 1H), 7.53 (s, 1H), 7.59 (s, 1H).

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 4 h
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water (2×20 mL), brine (10 mL)
  5. customdried
  6. concentrationconcentrated
  7. customThe crude product was purified by flash column chromatography

출처 및 근거

ORD 기록
ord-e0e3c810dfec45588051f6b01ba973c4
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722720B2

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