Diisobutylaluminumhydride → HCID 86679038、化合物

HRID 1907871ノート

反応式

HRID 1907871 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-ee963dbd0d0d410cb9fc46e4b7864d5b
出典データセット
uspto-grants-2013_12
特許番号
US08598189B2

反応ノート

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