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2-Cyclopenten-1-one → 3-(2-(4-(Benzo[D]thiazol-2-ylamino)phenoxy)pyridin-3-YL)cyclopent-2-enone

HRID 410300
ノート
印刷プレビュー

反応式

HRID 410300 の反応式
Br[C:2]1[C:3]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]3[S:17][C:18]4[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=4[N:20]=3)=[CH:11][CH:10]=2)=[N:4][CH:5]=[CH:6][CH:7]=1.[C:25]1(=[O:30])[CH2:29][CH2:28][CH:27]=[CH:26]1.CN(C1CCCCC1)C1CCCCC1>O1CCOCC1.CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[S:17]1[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=2[N:20]=[C:16]1[NH:15][C:12]1[CH:13]=[CH:14][C:9]([O:8][C:3]2[C:2]([C:27]3[CH2:28][CH2:29][C:25](=[O:30])[CH:26]=3)=[CH:7][CH:6]=[CH:5][N:4]=2)=[CH:10][CH:11]=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 59326883N-(4-(3-bromopyridin-2-yloxy)phenyl)benzo[d]thiazol-2-amine

生成物 1

HCID 462148733-(2-(4-(Benzo[D]thiazol-2-ylamino)phenoxy)pyridin-3-YL)cyclopent-2-enone

試薬・触媒・溶媒 2

HCID 178418851HCID 178418851、化合物触媒
HCID 31275
1,4-Dioxane
溶媒

反応条件

温度
90 °C

実験手順

A solution of N-(4-(3-bromopyridin-2-yloxy)phenyl)benzo[d]thiazol-2-amine (600 mg, 1.506 mmol), 2-cyclopenten-1-one (0.609 mL, 7.53 mmol), n-methyldicyclohexylamine (0.959 mL, 4.52 mmol) and bis(tri-tert-butylphosphine)palladium (0) (77 mg, 0.151 mmol) in Dioxane (4 mL) was capped, degassed and backfilled with argon. The reaction was heated to 90° C. After 6 h, the reaction was heated to 110° C. After 36 h, the reaction was cooled to 23° C., diluted with EtOAc (150 mL) and washed with water (100 mL) and brine (100 mL), dried over MgSO4, concentrated in vacuo and purified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane), affording the product as a yellow solid. MS (ESI, pos. ion) m/z: 400.1 (M+1).

後処理

  1. customdegassed
  2. temperaturethe reaction was heated to 110° C
  3. waitAfter 36 h
  4. temperaturethe reaction was cooled to 23° C.
  5. additiondiluted with EtOAc (150 mL)
  6. washwashed with water (100 mL) and brine (100 mL)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. custompurified by silica gel chromatography (eluant: 0.5-3% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-fc4f7fdfe855417bac3e67455f19af18
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759532B2

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