Ethyl Acetate → Salbutamol

HRID 1455721

반응식

HRID 1455721 반응식
[CH3:1][C:2]([NH:5][CH2:6][C@H:7]([OH:17])[C:8]1[CH:9]=[CH:10][C:11]([OH:16])=[C:12]([CH2:14][OH:15])[CH:13]=1)([CH3:4])[CH3:3].[ClH:18].C(OC(=O)C)C>CO>[CH3:4][C:2]([NH:5][CH2:6][CH:7]([OH:17])[C:8]1[CH:9]=[CH:10][C:11]([OH:16])=[C:12]([CH2:14][OH:15])[CH:13]=1)([CH3:1])[CH3:3].[CH3:4][C:2]([NH:5][CH2:6][C@H:7]([OH:17])[C:8]1[CH:9]=[CH:10][C:11]([OH:16])=[C:12]([CH2:14][OH:15])[CH:13]=1)([CH3:1])[CH3:3].[ClH:18]

참가 물질

5

반응물 2

HCID 8857Ethyl AcetateHCID 123601Levalbuterol Hydrochloride

생성물 2

HCID 2083SalbutamolHCID 123601Levalbuterol Hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a 2 L reactor equipped with a condenser, thermometer, and mechanical stirrer at 20° C. and under nitrogen, a suspension of wet levalbuterol hydrochloride (97.6 g), ethylacetate (440 mL) and methanol (49 mL) was formed. The suspension was stirred at 22° C.±2° C. for 4 hours. The solid was collected by filtration and washed with an ethylacetate:methanol mixture (90:10, 97 mL), and ethylacetate (2×97 mL). The product was dried at 22° C.±2° C. under vacuum (res. press. 40-45 mm Hg) for 24 hours to obtain 64.0 g (dry weight) in 92.5% yield from pure (R)-SLB.D-DBTA. The overall yield from racemic salbutamol to pure levalbuterol hydrochloride: 39.5%.

후처리

  1. customIn a 2 L reactor equipped with a condenser
  2. filtrationThe solid was collected by filtration
  3. washwashed with an ethylacetate
  4. customThe product was dried at 22° C.±2° C. under vacuum (res. press. 40-45 mm Hg) for 24 hours
  5. customto obtain
  6. custom64.0 g (dry weight) in 92.5% yield from pure (R)-SLB

출처 및 근거

ORD 기록
ord-34339f2b01244dfa8365eb04a1c578d4
출처 데이터셋
uspto-grants-2009_01
특허 번호
US07482489B2

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