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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
ノート
印刷プレビュー

反応式

HRID 2093645 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 23668039Potassium trimethylsilanolateHCID 595860421-{1-[5-(Trifluoromethyl)pyridin-2-yl]piperidin-4-yl}methanamine2 回HCID 68743634Methyl 4-[5-cyano-7-(1-fluoro-1-methylethyl)-1,3-benzoxazol-2-yl]benzoate

生成物 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

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-523839ed4b4146b69225f1beb9d6903a
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445480B2

反応ノート

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