ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Isobutanol → 4-[6-(8-Cyclopentyl-6-isobutoxy-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester

HRID 272432
ノート
印刷プレビュー

反応式

HRID 272432 の反応式
[H-].[Na+].[CH3:3][CH:4]([CH3:7])[CH2:5][OH:6].[C:8]([O:12][C:13]([N:15]1[CH2:20][CH2:19][N:18]([C:21]2[CH:22]=[N:23][C:24]([NH:27][C:28]3[N:29]=[CH:30][C:31]4[CH:37]=[C:36](F)[C:35](=[O:39])[N:34]([CH:40]5[CH2:44][CH2:43][CH2:42][CH2:41]5)[C:32]=4[N:33]=3)=[CH:25][CH:26]=2)[CH2:17][CH2:16]1)=[O:14])([CH3:11])([CH3:10])[CH3:9]>CCCCCC>[C:8]([O:12][C:13]([N:15]1[CH2:16][CH2:17][N:18]([C:21]2[CH:22]=[N:23][C:24]([NH:27][C:28]3[N:29]=[CH:30][C:31]4[CH:37]=[C:36]([O:6][CH2:5][CH:4]([CH3:7])[CH3:3])[C:35](=[O:39])[N:34]([CH:40]5[CH2:41][CH2:42][CH2:43][CH2:44]5)[C:32]=4[N:33]=3)=[CH:25][CH:26]=2)[CH2:19][CH2:20]1)=[O:14])([CH3:11])([CH3:9])[CH3:10]
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

5

反応物 3

HCID 6560IsobutanolHCID 24758Sodium hydrideHCID 114208294-[6-(8-Cyclopentyl-6-fluoro-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 112730084-[6-(8-Cyclopentyl-6-isobutoxy-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester収率 37%

試薬・触媒・溶媒 1

HCID 8058
Hexane
溶媒

反応条件

温度
95 °C

実験手順

60% Sodium hydride in oil (0.182 g, 4.4 mmol) was washed with hexane and added to 2-methyl-1-propanol (10 ml). This mixture effervesced and formed a solution. To this solution was added 4-[6-(8-cyclopentyl-6-fluoro-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester (0.225 g, 0.44 mmol, prepared as in Example 17) and the mixture was heated at 95° C. for 72 hours. The solvents were evaporated, and the residue was dissolved in diethyl ether then filtered. The filtrate was evaporated to provide 4-[6-(8-cyclopentyl-6-isobutoxy-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-ylamino)-pyridin-3-yl]-piperazine-1-carboxylic acid tert-butyl ester as a crystalline solid (0.092 g, 37%). MS (APCI) M++1: Calc'd, 564.3. Found 564.3.

後処理

  1. customformed a solution
  2. customThe solvents were evaporated
  3. dissolutionthe residue was dissolved in diethyl ether
  4. filtrationthen filtered
  5. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-987998efa7f04805b4f9ec69f34eb145
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07456168B2

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