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Oxalyl chloride → 4-[5-Cyano-7-(1-fluoro-1-methylethyl)-1,3-benzoxazol-2-yl]-N-({1-[5-(trifluoromethyl)pyridin-2-yl]piperidin-4-yl}methyl)benzamide

HRID 2093645
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HRID 2093645 반응식
[C:1]([C:3]1[CH:4]=[C:5]([C:22]([F:25])([CH3:24])[CH3:23])[C:6]2[O:10][C:9]([C:11]3[CH:20]=[CH:19][C:14]([C:15](OC)=[O:16])=[CH:13][CH:12]=3)=[N:8][C:7]=2[CH:21]=1)#[N:2].C[Si](C)(C)[O-].[K+].C(Cl)(=O)C(Cl)=O.[F:38][C:39]([F:55])([F:54])[C:40]1[CH:41]=[CH:42][C:43]([N:46]2[CH2:51][CH2:50][CH:49]([CH2:52][NH2:53])[CH2:48][CH2:47]2)=[N:44][CH:45]=1.C(N(C(C)C)CC)(C)C>O1CCCC1.CN(C)C=O.ClCCl>[C:1]([C:3]1[CH:4]=[C:5]([C:22]([F:25])([CH3:23])[CH3:24])[C:6]2[O:10][C:9]([C:11]3[CH:20]=[CH:19][C:14]([C:15]([NH:53][CH2:52][CH:49]4[CH2:50][CH2:51][N:46]([C:43]5[CH:42]=[CH:41][C:40]([C:39]([F:55])([F:54])[F:38])=[CH:45][N:44]=5)[CH2:47][CH2:48]4)=[O:16])=[CH:13][CH:12]=3)=[N:8][C:7]=2[CH:21]=1)#[N:2]
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참가 물질

9

반응물 5

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 23668039Potassium trimethylsilanolateHCID 595860421-{1-[5-(Trifluoromethyl)pyridin-2-yl]piperidin-4-yl}methanamine2회HCID 68743634Methyl 4-[5-cyano-7-(1-fluoro-1-methylethyl)-1,3-benzoxazol-2-yl]benzoate

생성물 1

HCID 25172491
4-[5-Cyano-7-(1-fluoro-1-methylethyl)-1,3-benzoxazol-2-yl]-N-({1-[5-(trifluoromethyl)pyridin-2-yl]piperidin-4-yl}methyl)benzamide

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of methyl 4-[5-cyano-7-(1-fluoro-1-methylethyl)-1,3-benzoxazol-2-yl]benzoate (29 mg, 0.086 mmol) in tetrahydrofuran (6 ml) at room temperature under nitrogen was added potassium trimethylsilanolate (36.7 mg, 0.257 mmol), and the resulting dark orange solution was stirred overnight. It was then concentrated in vacuo. To the residue was added dichloromethane (6 ml), oxalyl chloride (2M solution in dichloromethane) (0.257 ml, 0.514 mmol), and 1 drop of dimethylformamide. The mixture was stirred at room temperature for 1 h, and then concentrated in vacuo. To the residue was added tetrahydrofuran (6 ml), 1-{1-[5-(trifluoromethyl)pyridin-2-yl]piperidin-4-yl}methanamine (INTERMEDIATE 5, 33.3 mg, 0.129 mmol), and diisopropylethylamine (0.149 ml, 0.857 mmol). The reaction mixture was stirred at room temperature overnight, concentrated in vacuo, and purified by flash column chromatography. The recovered solid was triturated with hot methanol to afford the title compound. Mass spectrum (ESI) 566.2 (M+1). 1H NMR (500 MHz, CDCl3) δ: 8.38 (s, 1H), 8.32 (d, J=8.5 Hz, 2H), 8.04 (s, 1H), 7.95 (d, J=8.4 Hz, 2H), 7.76 (s, 1H), 7.61 (dd, J=2.5 Hz, J=9.2 Hz, 1H), 6.65 (d, J=9.2 Hz, 1H), 6.32 (t, J=5.9 Hz, 1H), 4.46 (d, J=13.4 Hz, 2H), 3.44 (t, J=6.4 Hz, 2H), 2.94 (m, 2H), 2.00 (m, 1H), 1.96 (s, 3H), 1.91 (s, 3H), 1.90 (br d, J=12.6 Hz, 2H), 1.34 (m, 2H).

후처리

  1. concentrationIt was then concentrated in vacuo
  2. stirringThe mixture was stirred at room temperature for 1 h
  3. concentrationconcentrated in vacuo
  4. stirringThe reaction mixture was stirred at room temperature overnight
  5. concentrationconcentrated in vacuo
  6. custompurified by flash column chromatography
  7. customThe recovered solid was triturated with hot methanol

출처 및 근거

ORD 기록
ord-523839ed4b4146b69225f1beb9d6903a
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445480B2

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