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Lithium Chloride → 3-(6-fluoropyridin-2-yl)-5-(pyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-c]pyridine

HRID 1775071
ノート
印刷プレビュー

反応式

HRID 1775071 の反応式
I[C:2]1[C:10]2[C:5](=[CH:6][N:7]=[C:8]([C:11]3[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=3)[CH:9]=2)[N:4]([CH2:17][O:18][CH2:19][CH2:20][Si:21]([CH3:24])([CH3:23])[CH3:22])[N:3]=1.[F:25][C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([Sn](CCCC)(CCCC)CCCC)[N:27]=1.[Li+].[Cl-]>CN(C=O)C.[Cu]I.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[F:25][C:26]1[N:27]=[C:28]([C:2]2[C:10]3[C:5](=[CH:6][N:7]=[C:8]([C:11]4[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=4)[CH:9]=3)[N:4]([CH2:17][O:18][CH2:19][CH2:20][Si:21]([CH3:24])([CH3:23])[CH3:22])[N:3]=2)[CH:29]=[CH:30][CH:31]=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

7

反応物 3

HCID 433294Lithium ChlorideHCID 164271152-Fluoro-6-(tributylstannyl)pyridineHCID 71253586HCID 71253586、化合物

生成物 1

HCID 712540573-(6-fluoropyridin-2-yl)-5-(pyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-c]pyridine収率 80%

試薬・触媒・溶媒 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 178418397HCID 178418397、化合物触媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

To a mixture of 3-iodo-5-(pyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-c]pyridine (GCP-P3-205-1) (200 mg, 0.44 mmol) and 2-fluoro-6-(tributylstannyl)pyridine (206 mg, 0.53 mmol) in 3 mL DMF, was added TEA 1 mL, LiCl (56 mg, 1.32 mmol) and CuI (84 mg, 0.44 mmol), and Pd(PPh3)4 (254 mg, 0.22 mmol). The reaction mixture was heated at 120° C. under microwave irradiation for 1 h, and the reaction was monitored by LCMS. Upon completion, the reaction mixture was extracted with 100 mL EtOAc, washed with 50 mL brine, and dried. The solvent was distilled off and the crude material was purified via flash chromatography, eluting with 5% to 30% ethyl acetate in heptane to afford 3-(6-fluoropyridin-2-yl)-5-(pyridin-3-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-c]pyridine as a yellow solid (148 mg, 80%). ESI MS m/z=421.1 (M+1).

後処理

  1. extractionUpon completion, the reaction mixture was extracted with 100 mL EtOAc
  2. washwashed with 50 mL brine
  3. customdried
  4. distillationThe solvent was distilled off
  5. customthe crude material was purified via flash chromatography
  6. washeluting with 5% to 30% ethyl acetate in heptane

出典と根拠

ORDレコード
ord-0f84ab7376ea431799c00c90f52dbb36
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09260425B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート