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Cesium carbonate → 4-[(2-cyclopentyl-4,4,6-trimethyl-5-oxo-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-10-yl)amino]-N-(1-ethyl-4-piperidyl)-2,5-difluoro-benzamide

HRID 2234316
ノート
印刷プレビュー

反応式

HRID 2234316 の反応式
Cl[C:2]1[N:12]=[C:11]2[C:5]([NH:6][C:7](=[O:20])[C:8]([CH3:19])([CH3:18])[CH2:9][N:10]2[CH:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[CH:4][N:3]=1.[NH2:21][C:22]1[C:38]([F:39])=[CH:37][C:25]([C:26]([NH:28][CH:29]2[CH2:34][CH2:33][N:32]([CH2:35][CH3:36])[CH2:31][CH2:30]2)=[O:27])=[C:24]([F:40])[CH:23]=1.[C:41](=O)([O-])[O-].[Cs+].[Cs+].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>[Pd+2].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.O1CCOCC1>[CH:13]1([N:10]2[CH2:9][C:8]([CH3:19])([CH3:18])[C:7](=[O:20])[N:6]([CH3:41])[C:5]3[C:11]2=[N:12][C:2]([NH:21][C:22]2[C:38]([F:39])=[CH:37][C:25]([C:26]([NH:28][CH:29]4[CH2:34][CH2:33][N:32]([CH2:35][CH3:36])[CH2:31][CH2:30]4)=[O:27])=[C:24]([F:40])[CH:23]=2)=[N:3][CH:4]=3)[CH2:17][CH2:16][CH2:15][CH2:14]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 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 581540122-Chloro-9-cyclopentyl-7,7-dimethyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one2 回HCID 686848474-amino-N-(1-ethyl-4-piperidyl)-2,5-difluoro-benzamide2 回

生成物 1

HCID 68686107
4-[(2-cyclopentyl-4,4,6-trimethyl-5-oxo-2,6,9,11-tetrazabicyclo[5.4.0]undeca-7,9,11-trien-10-yl)amino]-N-(1-ethyl-4-piperidyl)-2,5-difluoro-benzamide
収率 54.6%

試薬・触媒・溶媒 2

HCID 9897284tris(dibenzylideneacetone) palladium (II)触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

10-chloro-2-cyclopentyl-4,4-dimethyl-2,6,9,11-tetrazabicyclo[5.4.0]undeca-8,10,12-trien-5-one (Intermediate 127; 100 mg, 0.32 mmol), 4-amino-N-(1-ethyl-4-piperidyl)-2,5-difluoro-benzamide (Intermediate 235; 101 mg, 0.36 mmol) and caesium carbonate (22 mg, 0.65 mmol) added to dioxane (5 mL) and the suspension bubbled with nitrogen for 10 minutes. tris(dibenzylideneacetone) palladium (II) (18 mg, 0.02 mmol) and XANTPHOS (17 mg, 0.03 mmol) were added and the mixture heated at 110° C. overnight. The mixture was filtered and the filtrate loaded onto an SCX (10 g) cartridge pre-wet with methanol, washed with methanol and eluted with methanolic ammonia. Product containing fractions were combined and evaporated and the resultant material purified by base modified reverse phase preparative HPLC to yield the title compound as a white crystalline solid (97 mg, 54%).

後処理

  1. customthe suspension bubbled with nitrogen for 10 minutes
  2. filtrationThe mixture was filtered
  3. washwashed with methanol
  4. washeluted with methanolic ammonia
  5. additionProduct containing fractions
  6. customevaporated
  7. customthe resultant material purified by base modified reverse phase preparative HPLC

出典と根拠

ORDレコード
ord-ef8721cc84e9428b9152816b27b78891
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709471B2

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