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

Potassium Carbonate → tert-Butyl 4-(2-methyl-4-nitrophenyl)piperazine-1-carboxylate

HRID 1181618
ノート
印刷プレビュー

反応式

HRID 1181618 の反応式
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].[N:12]1([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[N:15]1[CH2:14][CH2:13][N:12]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16]1
参加物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 11430Potassium CarbonateHCID 68001Benzene, 1-fluoro-2-methyl-4-nitro-HCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 22336105tert-Butyl 4-(2-methyl-4-nitrophenyl)piperazine-1-carboxylate収率 62%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.65 g (3.10 mmol) of 2-fluoro-5-nitrotoluene, 6.71 g (3.60 mmol) of tert-butyl 1-piperazinecarboxylate and 10.4 g (7.50 mmol) of potassium carbonate are solubilized under an argon atmosphere, in dry DMF (50 ml), then the reaction medium is taken to 80° C. for 18 hours. The reaction medium is then cooled down using an ice bath then poured into ice-cold water. The product is extracted using 3 times 50 ml of ethyl acetate. The organic solution is dried over magnesium sulphate, followed by filtration and concentration under vacuum. Purification is then carried out by crystallization from diisopropyl ether and the solid obtained is filtered and rinsed with isopentane in order to obtain, after drying, 5.9 g of a yellow solid product (yield 62%). Melting point: 121.8-123.4° C.

後処理

  1. temperatureThe reaction medium is then cooled down
  2. additionthen poured into ice-cold water
  3. extractionThe product is extracted
  4. dry with materialThe organic solution is dried over magnesium sulphate
  5. filtrationfollowed by filtration and concentration under vacuum
  6. customPurification
  7. customis then carried out by crystallization from diisopropyl ether
  8. customthe solid obtained
  9. filtrationis filtered
  10. washrinsed with isopentane in order
  11. customto obtain
  12. customafter drying

出典と根拠

ORDレコード
ord-b1bbe7d7e7304ccbbcef895c9a6e3649
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07285664B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート