4-Bromoaniline → HCID 13221932、化合物

HRID 1472821ノート

反応式

HRID 1472821 の反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[N:9]1([CH:14]([CH3:18])[C:15](O)=[O:16])[CH2:13][CH2:12][CH2:11][CH2:10]1.C(N(C(C)C)CC)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CC(N(C)C)=O.O>[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:15](=[O:16])[CH:14]([N:9]2[CH2:13][CH2:12][CH2:11][CH2:10]2)[CH3:18])=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 78074-BromoanilineHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 31571772-(Pyrrolidin-1-yl)propanoic acid

生成物 1

HCID 13221932HCID 13221932、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

4-Bromo aniline (0.25 g, 1.45 mmol), 2-pyrrolidin-1-ylpropanoic acid (0.25 g, 1.74 mmol) and diisopropylethylamine (0.3 ml, 1.74 mmol) were dissolved in dimethylacetamide (5 ml). HBTU (0.66 g, 1.74 mmol) was subsequently added and the mixture was stirred overnight. The reaction mixture was added to water and extracted twice with ethyl acetate. The combined organics were washed several times with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give the desired product. Yield: 0.43 g, 100%. LCMS method: 2, RT: 2.73 min; MI: 297-299 [M+1].

後処理

  1. extractionextracted twice with ethyl acetate
  2. washThe combined organics were washed several times with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e7f9a3d3964f49e3aff55599e70f4088
出典データセット
uspto-grants-2015_04
特許番号
US09012633B2

反応ノート

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