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Hydrogen Bromide → Terbutaline

HRID 1578632
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HRID 1578632 반응식
Br.C([O:5][C:6]1[CH:7]=[C:8]([CH:16]([OH:23])[CH2:17][NH:18][C:19]([CH3:22])([CH3:21])[CH3:20])[CH:9]=[C:10]([O:12]C(=O)C)[CH:11]=1)(=O)C.O.CCOCC>C(O)C.[Pd]>[OH:5][C:6]1[CH:7]=[C:8]([CH:16]([OH:23])[CH2:17][NH:18][C:19]([CH3:21])([CH3:20])[CH3:22])[CH:9]=[C:10]([OH:12])[CH:11]=1
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참가 물질

7

반응물 4

HCID 260Hydrogen BromideHCID 962WaterHCID 3283Diethyl EtherHCID 21450028HCID 21450028, 화합물

생성물 1

HCID 5403Terbutaline

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol
용매

실험 절차

1.1 g of this salt were dissolved in warm absolute ethanol and 0.1 g 10% palladium charcoal were added. The solution was then hydrogenated at 50°C. and 5 atmospheres pressure overnight. The catalyst was filtered off and the volume of the solution reduced by evaporation. The hydrobromide of 1-(3',5'-diacetoxyphenyl)-2-(t-butylamino)-ethanol with 1 mole of water was precipitated by the addition of ether. M.p. 108°-111°C. The protective acetyl groups may be removed by boiling the 1-(3',5'-diacetoxyphenyl)-2-(t-butylamino)-ethanol hydrobromide with 1% hydrobromic acid for three hours. After evaporation and drying the product was recrystallized as described in Example 2c.

후처리

  1. customwas then hydrogenated at 50°C.
  2. custom5 atmospheres pressure overnight
  3. filtrationThe catalyst was filtered off
  4. customthe volume of the solution reduced by evaporation
  5. customThe protective acetyl groups may be removed
  6. customfor three hours
  7. customAfter evaporation
  8. customdrying the product
  9. customwas recrystallized

출처 및 근거

ORD 기록
ord-4bf788f4a52546c5a3c6af9d21f00452
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03937838

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