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Dichloromethane → 2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-6-(5-methyl-1H-pyrazol-4-yl)-5H-pyrrolo[2,3-b]pyrazine

HRID 1052313
ノート
印刷プレビュー

反応式

HRID 1052313 の反応式
Br[C:2]1[N:24](S(C2C=CC=CC=2)(=O)=O)[C:5]2=[N:6][CH:7]=[C:8]([CH2:10][CH2:11][C:12]3[C:17]([F:18])=[C:16]([O:19][CH3:20])[CH:15]=[C:14]([O:21][CH3:22])[C:13]=3[F:23])[N:9]=[C:4]2[CH:3]=1.[CH3:34][C:35]1[C:39](B(O)O)=[CH:38][NH:37][N:36]=1.ClCCl.P([O-])([O-])([O-])=O.[K+].[K+].[K+].C(=O)([O-])[O-].[K+].[K+]>O.Cl[Pd]Cl.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2].O1CCOCC1>[F:18][C:17]1[C:16]([O:19][CH3:20])=[CH:15][C:14]([O:21][CH3:22])=[C:13]([F:23])[C:12]=1[CH2:11][CH2:10][C:8]1[N:9]=[C:4]2[CH:3]=[C:2]([C:39]3[CH:38]=[N:37][NH:36][C:35]=3[CH3:34])[NH:24][C:5]2=[N:6][CH:7]=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

9

反応物 5

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 62657Potassium Phosphate, TribasicHCID 899635876-bromo-2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-5-(phenylsulfonyl)-5H-pyrrolo[2,3-b]pyrazineHCID 178434488HCID 178434488、化合物

生成物 1

HCID 73054235
2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-6-(5-methyl-1H-pyrazol-4-yl)-5H-pyrrolo[2,3-b]pyrazine
収率 46%

試薬・触媒・溶媒 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)触媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
88 °C

実験手順

A stirred mixture of 6-bromo-2-[2-(2,6-difluoro-3,5-dimethoxyphenyl)ethyl]-5-(phenylsulfonyl)-5H-pyrrolo[2,3-b]pyrazine (15 mg, 28 μmol), (3-methyl-1H-pyrazol-4-yl)boronic acid (4.2 mg, 33 μmol), [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) complexed with dichloromethane (1:1) (1.8 mg, 2.2 μmol), and potassium phosphate (9.5 mg, 45 mmol) in water (0.2 mL)/1,4-dioxane (1 mL) was heated at 88° C. After 1 hour, the volatiles were removed under vacuum and the residue was dissolved in methanol (1 mL). Potassium carbonate (7.7 mg, 56 μmol) was added and the reaction mixture was warmed up to 60° C. After 0.5 hour, the reaction mixture was cooled to ambient temperature and was purified on RP-HPLC (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min) to give the desired product (5.1 mg, 46%) as its TFA salt. LCMS calculated for C20H20F2N5O2 (M+H)+: m/z=400.2. Found: 400.2.

後処理

  1. customthe volatiles were removed under vacuum
  2. dissolutionthe residue was dissolved in methanol (1 mL)
  3. temperaturethe reaction mixture was warmed up to 60° C
  4. waitAfter 0.5 hour
  5. temperaturethe reaction mixture was cooled to ambient temperature
  6. customwas purified on RP-HPLC (XBridge C18 column
  7. washeluting with a gradient of acetonitrile/water containing 0.05% TFA, at flow rate of 30 mL/min)

出典と根拠

ORDレコード
ord-5c060d9a9eee4f50a3582977c518e727
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388185B2

反応ノート

読み込み中…

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