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Dichloromethane → 2-Chloro-4-[5-fluoro-4-(1-hydroxy-ethyl)-pyridin-3-yl]-benzonitrile

HRID 1897588
ノート
印刷プレビュー

反応式

HRID 1897588 の反応式
[Cl:1][C:2]1[CH:9]=[C:8](B2OC(C)(C)C(C)(C)O2)[CH:7]=[CH:6][C:3]=1[C:4]#[N:5].Br[C:20]1[CH:21]=[N:22][CH:23]=[C:24]([F:29])[C:25]=1[CH:26]([OH:28])[CH3:27].C(Cl)Cl.C([O-])([O-])=O.[Na+].[Na+]>CN(C=O)C.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:1][C:2]1[CH:9]=[C:8]([C:20]2[CH:21]=[N:22][CH:23]=[C:24]([F:29])[C:25]=2[CH:26]([OH:28])[CH3:27])[CH:7]=[CH:6][C:3]=1[C:4]#[N:5]
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

7

反応物 4

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 579261132-Chloro-4-(tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrileHCID 699379091-(3-Bromo-5-Fluoro-pyridin-4-yl)-ethanol

生成物 1

HCID 710875962-Chloro-4-[5-fluoro-4-(1-hydroxy-ethyl)-pyridin-3-yl]-benzonitrile収率 49.9%

試薬・触媒・溶媒 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

To the solution of 2-Chloro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-benzonitrile (263 mg, 1.00 mmol), 1-(3-Bromo-5-Fluoro-pyridin-4-yl)-ethanol (220 mg, 1.00 mmol) and PdCl2(dppf). CH2Cl2 adduct (65 mg, 0.08 mmol) in DMF (4 mL) was added 2M Na2CO3 solution (1.50 ml, 3.00 mmol) under nitrogen atmosphere. The mixture was stirred and heated at 100° C. for 4 hrs. After letting cool to room temperature, solvent was removed in vacuo. The resulting residue was dissolved in DCM and sat. NH4Cl solution. After extraction with DCM, the combined extracts were concentrated and purified by ISCO 12 g (0-30% EtOAc/Hep) to give 2-Chloro-4-[5-fluoro-4-(1-hydroxy-ethyl)-pyridin-3-yl]-benzonitrile (138 mg, 49%) as a white solid; ESI-MS m/z: 276 [M+1]+, Retention time 1.15 min. 1H-NMR (CDCl3, 400 MHz) δ 1.53 (d, J=6.8 Hz, 3H), 4.76 (q, J=6.8 Hz, 1H), 7.28 (dd, J=8.0, 2.0 Hz, 1H), 7.45 (d, J=2.0 Hz, 1H), 7.71 (d, J=8.0 Hz, 1H), 8.20 (s, 1H), 8.46 (d, J=2.0 Hz, 1H). The racemate was separated by chiral HPLC (ChiralPak IA-H, 40% EtOH/Heptane, v/v) and yielded 2-Chloro-4-[5-fluoro-4-((R)-1-hydroxy-ethyl)-pyridin-3-yl]-benzonitrile 16-(enantiomer-1) (retention time: 5.24 min) and 2-Chloro-4-[5-fluoro-4-((S)-1-hydroxy-ethyl)-pyridin-3-yl]-benzonitrile 16-(enantiomer-2) (retention time: 13.69 min).

後処理

  1. temperatureAfter letting cool to room temperature
  2. customsolvent was removed in vacuo
  3. dissolutionThe resulting residue was dissolved in DCM
  4. extractionAfter extraction with DCM
  5. concentrationthe combined extracts were concentrated
  6. custompurified by ISCO 12 g (0-30% EtOAc/Hep)

出典と根拠

ORDレコード
ord-09a6f20fd9ae4686be6256cc92cf219e
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08519134B2

反応ノート

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