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Dicyclohexylcarbodiimide → HCID 21918641、化合物

HRID 1250070
ノート
印刷プレビュー

反応式

HRID 1250070 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-:3])=[O:2].[C:16]([C:20]1[CH:21]=[C:22]([CH:26]=[C:27]([C:30]([CH3:33])([CH3:32])[CH3:31])[C:28]=1[OH:29])[C:23](O)=[O:24])([CH3:19])([CH3:18])[CH3:17].C1(N=C=NC2CCCCC2)CCCCC1>CN(C=O)C>[CH3:33][C:30]([C:27]1[CH:26]=[C:22]([C:23]([N:13]2[CH2:14][CH2:15][N:10]([C:7]3[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=3)[CH2:11][CH2:12]2)=[O:24])[CH:21]=[C:20]([C:16]([CH3:19])([CH3:18])[CH3:17])[C:28]=1[OH:29])([CH3:31])[CH3:32]
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 10868DicyclohexylcarbodiimideHCID 150073,5-Di-tert-butyl-4-hydroxybenzoic acidHCID 804471-(4-Nitrophenyl)piperazine

生成物 1

HCID 21918641HCID 21918641、化合物収率 89%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2.07 g (10 mmoles) of 1-(4-nitrophenyl)piperazine, 2.5 g (10 mmoles) of 3,5-di-tert-butyl-4-hydroxybenzoic acid and 2.26 g (11 mmoles) of dicyclohexylcarbodiimide are introduced into a 100 ml flask containing 25 ml of DMF. The reaction medium is agitated for 15 hours at ambient temperature, the precipitate which appears is filtered out and rinsed with ethyl acetate. After concentration of the filtrate under reduced pressure, the residue is diluted in 20 ml of ethyl acetate and a new insoluble is eliminated by filtration. The solvent is evaporated off under vacuum and the residue is precipitated from diethyl ether. The solid is filtered, rinsed with 2×20 ml of ethyl acetate in order to obtain a yellow powder with a yield of 89%. Melting point: 159.5-160.5° C.

後処理

  1. filtrationthe precipitate which appears is filtered out
  2. washrinsed with ethyl acetate
  3. additionAfter concentration of the filtrate under reduced pressure, the residue is diluted in 20 ml of ethyl acetate
  4. filtrationa new insoluble is eliminated by filtration
  5. customThe solvent is evaporated off under vacuum
  6. customthe residue is precipitated from diethyl ether
  7. filtrationThe solid is filtered
  8. washrinsed with 2×20 ml of ethyl acetate in order
  9. customto obtain a yellow powder with a yield of 89%

出典と根拠

ORDレコード
ord-301c6b42dbf042a6b60c278ad6258859
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06335445B1

反応ノート

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