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Triethylamine → HCID 57591440、化合物

HRID 1784144
ノート
印刷プレビュー

反応式

HRID 1784144 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([NH:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[CH2:24]([O:31][C:32](=[O:43])[CH:33]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:34](O)=[O:35])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(CC)CC>CN(C=O)C>[CH2:24]([O:31][C:32](=[O:43])[CH:33]([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:34]([N:11]([C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([F:22])([F:21])[F:23])=[CH:16][CH:15]=1)=[O:35])[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 117278Propanedioic acid, 2-phenyl-, 1-(phenylmethyl) esterHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 57591499HCID 57591499、化合物

生成物 1

HCID 57591440HCID 57591440、化合物収率 29%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of 0.7 g (2.1 mmol) (3,4-Dimethoxy-phenyl)-[2-(4-trifluoromethyl-phenyl)-ethyl]-amine, 0.58 g (2.1 mmol) 2-phenyl-malonic acid monobenzylester (commercially available), 0.83 g (2.5 mmol) TBTU and 0.43 g (4.3 mmol) NEt3 in 15 mL DMF was stirred at room temperature for 16 h. After evaporation to dryness the residue was treated with HCl aq. and DCM. The combined organic phases were washed with HCl aq., dried with MgSO4 and evaporated to dryness. The residue was purified by flash column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane. The product containing fractions were combined and evaporated to dryness to yield 0.35 g (29%) of the title compound. MS(m/e): 578.3 (MH+).

後処理

  1. customAfter evaporation to dryness the residue
  2. additionwas treated with HCl aq. and DCM
  3. washThe combined organic phases were washed with HCl aq.
  4. dry with materialdried with MgSO4
  5. customevaporated to dryness
  6. customThe residue was purified by flash column chromatography on silica eluting with a gradient
  7. customformed from ethyl acetate and heptane
  8. additionThe product containing fractions
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-b788071888c243319146f7e8d516f378
出典データセット
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07501541B2

反応ノート

読み込み中…

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