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Thionyl Chloride → [2-(3-Chloro-4-fluoro-phenoxy)-pyridin-3-yl]-(6-methyl-3,4-dihydro-2H-quinolin-1-yl)-methanone

HRID 1877365
ノート
印刷プレビュー

反応式

HRID 1877365 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][C:17]=1[F:18])[O:5][C:6]1[N:14]=[CH:13][CH:12]=[CH:11][C:7]=1[C:8]([OH:10])=O.S(Cl)(Cl)=O.C(N(C(C)C)C(C)C)C.[CH3:32][C:33]1[CH:34]=[C:35]2[C:40](=[CH:41][CH:42]=1)[NH:39][CH2:38][CH2:37][CH2:36]2>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][C:17]=1[F:18])[O:5][C:6]1[C:7]([C:8]([N:39]2[C:40]3[C:35](=[CH:34][C:33]([CH3:32])=[CH:42][CH:41]=3)[CH2:36][CH2:37][CH2:38]2)=[O:10])=[CH:11][CH:12]=[CH:13][N:14]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 24386Thionyl ChlorideHCID 666786-Methyl-1,2,3,4-tetrahydroquinolineHCID 81531DiisopropylethylamineHCID 128493372-(3-Chloro-4-fluoro-phenoxy)-nicotinic acid

生成物 1

HCID 46194846[2-(3-Chloro-4-fluoro-phenoxy)-pyridin-3-yl]-(6-methyl-3,4-dihydro-2H-quinolin-1-yl)-methanone収率 8%

反応条件

温度
140 °C

実験手順

A solution of 2-(3-chloro-4-fluoro-phenoxy)-nicotinic acid (32.1 mg, 0.12 mmol, 1.0 equiv) in thionyl chloride (57 mg, 35 pt, 0.48 mmol, 4.0 equiv; [CAS RN 7719-09-7]) was stirred at rt for 1 h. The reaction mixture was concentrated under reduced pressure, remaining thionyl chloride removed by azotropic distillation with toluene and the residue dissolved in anhydrous DMF (1 mL). To this solution was added N-ethyldiisopropylamine (77.6 mg, 102 μL, 0.60 mmol, 5.0 equiv; [CAS RN 7087-68-5]) and 6-methyl-1,2,3,4-tetrahydro-quinoline (21.2 mg, 0.14 mmol, 1.2 equiv; [CAS RN 91-61-2]) and the reaction mixture heated by microwave irradiation to 140° C. for 15 min. Removal of the solvent mixture under reduced pressure and purification by preparative HPLC on reversed phase (Xterra® PrepMSC 18, 5 μm, 19×50 mm column equipped with a Gilson Liquid Handler 215 auto sampler, two Rainin Dynamax® SD-300 pumps, a Sedex ELSD 75 lightscatter and a Dionex UVD 340S UV detector) eluting with a gradient of acetonitrile/water provided 3.7 mg (8%) of the title compound. MS (ISP): 397.0 [M+H]+.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customremoved by azotropic distillation with toluene
  3. dissolutionthe residue dissolved in anhydrous DMF (1 mL)
  4. customRemoval of the solvent mixture
  5. customunder reduced pressure and purification by preparative HPLC on reversed phase (Xterra® PrepMSC 18, 5 μm, 19×50 mm column
  6. customequipped with a Gilson Liquid Handler 215 auto sampler, two Rainin Dynamax® SD-300 pumps
  7. washa Sedex ELSD 75 lightscatter and a Dionex UVD 340S UV detector) eluting with a gradient of acetonitrile/water

出典と根拠

ORDレコード
ord-66b4f6a604a04b68a59d1263a874b722
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309734B2

反応ノート

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