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Diisopropylethylamine → HCID 71525480、化合物

HRID 1477765
ノート
印刷プレビュー

反応式

HRID 1477765 の反応式
Br[C:2]1[N:3]=[CH:4][C:5]([C:15]([OH:17])=O)=[N:6][C:7]=1[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=1.Cl[C:19](N(C)C)=[C:20]([CH3:22])C.Cl.[CH3:27][C:28]([CH3:36])([C:30]1[N:34]=[C:33]([CH3:35])[O:32][N:31]=1)[NH2:29].C(N(C(C)C)C(C)C)C>ClCCl.CN(C=O)C>[CH3:27][C:28]([NH:29][C:15]([C:5]1[CH:4]=[N:3][C:2]([CH:22]2[CH2:20][CH2:19]2)=[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=2)[N:6]=1)=[O:17])([C:30]1[N:34]=[C:33]([CH3:35])[O:32][N:31]=1)[CH3:36]
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 81531DiisopropylethylamineHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 470030732-(5-Methyl-1,2,4-oxadiazol-3-yl)propan-2-amine hydrochlorideHCID 86682316HCID 86682316、化合物

生成物 1

HCID 71525480HCID 71525480、化合物収率 49.6%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 6344Dichloromethane溶媒

実験手順

5-Bromo-6-(3-chloro-phenyl)-pyrazine-2-carboxylic acid (0.200 g, 638 μmol) was suspended in dichloromethane (1 mL) and 1-chloro-N,N,2-trimethylpropenylamine (98.0 mg, 97.0 μl, 734 μmol) was added dropwise at room temperature. After 30 min stirring the brown solution was added drop by drop to a solution of α,α,5-trimethyl-1,2,4-oxadiazole-3-methanamine hydrochloride (CAN 1240526-27-5; 142 mg, 797 μmol) and ethyldiisopropylamine (206 mg, 264 μl, 1.59 mmol) in DMF (1 mL) and the reaction mixture was stirred at room temperature for 30 minutes. The mixture was extracted with ethyl acetate and 1M citric acid solution; the organic phase was dried with MgSO4; filtered and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 20 g, 5% to 50% ethyl acetate in n-heptane) to give the desired product (126 mg, 45%) as white foam; MS (EI): 436.0 (M+H).

後処理

  1. stirringthe reaction mixture was stirred at room temperature for 30 minutes
  2. extractionThe mixture was extracted with ethyl acetate and 1M citric acid solution
  3. dry with materialthe organic phase was dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by flash chromatography (silica gel, 20 g, 5% to 50% ethyl acetate in n-heptane)

出典と根拠

ORDレコード
ord-c2cf52f4c5484dd4ae70a9bf0df57be1
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09403808B2

反応ノート

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