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2-Cyclopenten-1-one → 3-(2-(4-(Pyridin-2-ylamino)phenoxy)pyridin-3-yl)cyclopent-2-enone

HRID 473664
ノート
印刷プレビュー

反応式

HRID 473664 の反応式
Cl.Br[C:3]1[C:4]([O:9][C:10]2[CH:15]=[CH:14][C:13]([NH:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)=[CH:12][CH:11]=2)=[N:5][CH:6]=[CH:7][CH:8]=1.CN(C1CCCCC1)C1CCCCC1.[C:37]1(=[O:42])[CH2:41][CH2:40][CH:39]=[CH:38]1>O1CCOCC1.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>[N:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[NH:16][C:13]1[CH:14]=[CH:15][C:10]([O:9][C:4]2[C:3]([C:39]3[CH2:40][CH2:41][C:37](=[O:42])[CH:38]=3)=[CH:8][CH:7]=[CH:6][N:5]=2)=[CH:11][CH:12]=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

6

反応物 3

HCID 135882-Cyclopenten-1-oneHCID 24210N-Methyl dicyclohexylamineHCID 67425919N-(4-(3-Bromopyridin-2-yloxy)phenyl)pyridin-2-amine hydrochloride

生成物 1

HCID 593739783-(2-(4-(Pyridin-2-ylamino)phenoxy)pyridin-3-yl)cyclopent-2-enone

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒
HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
23 °C

実験手順

A suspension of N-(4-(3-bromopyridin-2-yloxy)phenyl)pyridin-2-amine hydrochloride (600 mg, 1.585 mmol) in Dioxane (4 mL) was treated with n-methyldicyclohexylamine (1.008 mL, 4.75 mmol, 3.0 equiv). The reaction was stirred at 23° C. for 15 min, followed by the addition of 2-cyclopenten-1-one (0.641 mL, 7.92 mmol, 5.0 equiv) and bis(tri-tert-butylphosphine)palladium (0) (81 mg, 0.158 mmol, 0.1 equiv). The reaction vessel was capped, degassed and backfilled with argon, and heated at 105° C. After 6 h, the reaction was cooled to 23° C., diluted with EtOAc (100 mL) and washed with water (75 mL) and brine (75 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane), affording 3-(2-(4-(pyridin-2-ylamino)phenoxy)pyridin-3-yl)cyclopent-2-enone. MS (ESI, pos. ion) m/z: 344.1 (M+1). IC50 (uM) 0.015.

後処理

  1. customThe reaction vessel was capped
  2. customdegassed
  3. temperatureheated at 105° C
  4. waitAfter 6 h
  5. temperaturethe reaction was cooled to 23° C.
  6. additiondiluted with EtOAc (100 mL)
  7. washwashed with water (75 mL) and brine (75 mL)
  8. dry with materialdried over MgSO4
  9. concentrationconcentrated in vacuo
  10. custompurified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-0b7724e61c714c77881e81729c1791d6
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08637500B2

反応ノート

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