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Diisopropylethylamine → HCID 23121832、化合物

HRID 1713549
ノート
印刷プレビュー

反応式

HRID 1713549 の反応式
[NH2:1][C:2]1[C:10]2[N:9]=[CH:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(N(C(C)C)CC)(C)C.Cl[C:28](OC1C=CC([N+]([O-])=O)=CC=1)=[O:29].[C:40]1([C:46]2([C:56]3[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=3)[CH:50]3[CH2:51][NH:52][CH2:53][CH2:54][N:49]3[C:48](=[O:55])[O:47]2)[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1>O1CCCC1.C(OCC)(=O)C>[O:55]=[C:48]1[N:49]2[CH2:54][CH2:53][N:52]([C:28]([NH:1][C:2]3[C:10]4[N:9]=[CH:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[C:6]=4[CH:5]=[CH:4][CH:3]=3)=[O:29])[CH2:51][CH:50]2[C:46]([C:40]2[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=2)([C:56]2[CH:57]=[CH:58][CH:59]=[CH:60][CH:61]=2)[O:47]1
参加物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 81531Diisopropylethylamine2 回HCID 821294-Nitrophenyl chloroformateHCID 18355224tert-butyl 4-amino-1H-benzo[d]imidazole-1-carboxylateHCID 231218811,1-Diphenyltetrahydro-1H-oxazolo[3,4-a]pyrazin-3(5H)-one

生成物 1

HCID 23121832HCID 23121832、化合物収率 66.2%

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1,1-dimethylethyl 4-amino-1H-benzimidazole-1-carboxylate (0.12 g, 0.50 mmol) in tetrahydrofuran (10 ml) were added diisopropylethylamine (90 μL, 0.50 mmol) and 4-nitrophenyl chloroformate (0.11 g, 0.50 mmol), and the mixture was stirred at room temperature for 4 hours. Hexahydro-1,1-diphenyl-3H-oxazolo[3,4-a]pyrazin-3-one (88 mg, 0.30 mmol) and diisopropylethylamine (90 μL, 0.50 mmol) were sequentially added thereto, and the mixture was stirred at room temperature overnight. To the reaction solution were added ethyl acetate (50 mL) and a 0.5 M aqueous sodium hydrogen carbonate solution (50 mL), and the obtained crystals were collected by filtration. The crude crystals were sequentially washed with a 0.5 M aqueous sodium hydrogen carbonate solution, water and ethyl acetate to obtain the title compound (0.11 g, yield 65%).

後処理

  1. stirringthe mixture was stirred at room temperature overnight
  2. filtrationa 0.5 M aqueous sodium hydrogen carbonate solution (50 mL), and the obtained crystals were collected by filtration
  3. washThe crude crystals were sequentially washed with a 0.5 M aqueous sodium hydrogen carbonate solution, water and ethyl acetate

出典と根拠

ORDレコード
ord-e96e984172474199a9b694d2934f0013
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795267B2

反応ノート

読み込み中…

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