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Benzhydrylidene-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-amine → 4-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenylamine

HRID 403490
ノート
印刷プレビュー

反応式

HRID 403490 の反応式
C(=[N:14][C:15]1[CH:20]=[CH:19][C:18]([CH2:21][C:22]2[C:23]([CH2:33][CH3:34])=[N:24][N:25]3[C:30]([CH3:31])=[CH:29][C:28]([CH3:32])=[N:27][C:26]=23)=[CH:17][CH:16]=1)(C1C=CC=CC=1)C1C=CC=CC=1>O.CCO.Cl>[CH2:33]([C:23]1[C:22]([CH2:21][C:18]2[CH:17]=[CH:16][C:15]([NH2:14])=[CH:20][CH:19]=2)=[C:26]2[N:27]=[C:28]([CH3:32])[CH:29]=[C:30]([CH3:31])[N:25]2[N:24]=1)[CH3:34]
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 1

HCID 86671753Benzhydrylidene-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-amine

生成物 1

HCID 683791594-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenylamine

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Benzhydrylidene-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenyl]-amine (12) (3.97 g, 8.93 mmol) was dissolved in a mixture of water (40 ml), EtOH (10 ml) and conc. HCl (10 ml) and stirred at rt for 1 h. The reaction mixture was basified to pH 11 with Na2 CO3. The organic layer was extracted with EtOAc, washed with water and brine, dried over Na2 SO4 and concentrated to afford an orange oil. The crude product was purified by chromatography (2-50% EtOAc in cyclohexane) to afford a yellow solid.

後処理

  1. extractionThe organic layer was extracted with EtOAc
  2. washwashed with water and brine
  3. customdried over Na2 SO4
  4. concentrationconcentrated
  5. customto afford an orange oil
  6. customThe crude product was purified by chromatography (2-50% EtOAc in cyclohexane)
  7. customto afford a yellow solid

出典と根拠

ORDレコード
ord-d6ff6f2163364cec8b9e6602626960e0
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08748435B2

反応ノート

読み込み中…

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