Diisobutylaluminumhydride → HCID 86679038, 화합물

HRID 1853446노트

반응식

HRID 1853446 반응식
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

참가 물질

4

반응물 2

HCID 21225700DiisobutylaluminumhydrideHCID 68436940HCID 68436940, 화합물

생성물 1

HCID 86679038HCID 86679038, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4fddc36bfedb40f9b990c33623b198aa
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962644B2

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