Ethyl Acetate → 2-(6-Aminopyridin-3-yl)propan-2-ol

HRID 600629노트

반응식

HRID 600629 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:5](C(OC)=O)=[CH:4][N:3]=1.[CH3:12][Mg]Cl.[Cl-].[NH4+].C([O:20][CH2:21][CH3:22])(=O)C>C1COCC1>[NH2:1][C:2]1[N:3]=[CH:4][C:5]([C:21]([OH:20])([CH3:22])[CH3:12])=[CH:10][CH:11]=1

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 25517Ammonium ChlorideHCID 737487Methyl 6-aminonicotinateHCID 178418332HCID 178418332, 화합물

생성물 1

HCID 594737712-(6-Aminopyridin-3-yl)propan-2-ol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 0.7 g of methyl 6-aminonicotinate in 65 mL of THF, cooled to 10° C. and under argon, are added dropwise 15 mL of a 3M solution of methylmagnesium chloride in THF. The reaction mixture is stirred for 15 hours, while allowing the temperature to rise to 20° C., and is then cooled again in an ice bath. 100 mL of saturated ammonium chloride solution and then 200 mL of ethyl acetate are added slowly. The organic phase is dried and concentrated to dryness. The residue is taken up in ethyl acetate. The precipitate is filtered off by suction and dried to give 0.4 g of 2-(6-aminopyridin-3-yl)propan-2-ol in the form of a pale yellow solid.

후처리

  1. customto rise to 20° C.
  2. temperatureis then cooled again in an ice bath
  3. customThe organic phase is dried
  4. concentrationconcentrated to dryness
  5. filtrationThe precipitate is filtered off by suction
  6. customdried

출처 및 근거

ORD 기록
ord-13ab20eb2c00429ab4850ab6beff6d24
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902219B2

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