Diisobutylaluminumhydride → HCID 86679038、化合物

HRID 2202423ノート

反応式

HRID 2202423 の反応式
C[O:2][C:3]([C:5]1[CH:10]=[N:9][C:8]([NH:11][CH2:12][CH2:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)=[CH:7][N:6]=1)=O.[H-].C([Al+]CC(C)C)C(C)C>C(Cl)Cl>[CH3:21][N:18]1[CH2:19][CH2:20][CH:15]([CH2:14][CH2:13][CH2:12][NH:11][C:8]2[N:9]=[CH:10][C:5]([CH:3]=[O:2])=[N:6][CH:7]=2)[CH2:16][CH2:17]1

参加物

4

反応物 2

HCID 21225700DiisobutylaluminumhydrideHCID 68436940HCID 68436940、化合物

生成物 1

HCID 86679038HCID 86679038、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A −78° C. solution of 5-[3-(1-methyl-piperidin-4-yl)-propylamino]-pyrazine-2-carboxylic acid methyl ester in DCM (0.1 M) was treated with diisobutylaluminum hydride (1 M in hexanes; 1 equiv.) dropwise. The reaction was quenched with 1 M H2SO4, neutralized with satd. aq. NaHCO3, and diluted with MeOH, CHCl3, and satd. aq. sodium potassium tartrate. The mixture was stirred vigourously until the layers separated. The organic layer was dried (Na2SO4) and concentrated to give the crude product, which was used in the next step without further purification.

後処理

  1. customThe reaction was quenched with 1 M H2SO4
  2. additionaq. NaHCO3, and diluted with MeOH, CHCl3
  3. customseparated
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-beeab08db12d43a58b14f6e63c67e176
出典データセット
uspto-grants-2016_06
特許番号
US09365548B2

反応ノート

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