Ethanol → Amosulalol

HRID 1855960노트

반응식

HRID 1855960 반응식
[OH:1][CH:2]([C:23]1[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([S:29]([NH2:32])(=[O:31])=[O:30])[CH:28]=1)[CH2:3][N:4]([CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][CH3:22])CC1C=CC=CC=1.C(O)C>CO.[H][H].[Pd]>[OH:1][CH:2]([C:23]1[CH:24]=[CH:25][C:26]([CH3:33])=[C:27]([S:29]([NH2:32])(=[O:30])=[O:31])[CH:28]=1)[CH2:3][NH:4][CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[O:21][CH3:22]

참가 물질

6

반응물 2

HCID 702EthanolHCID 133583145-(2-{Benzyl[2-(2-methoxyphenoxy)ethyl]amino}-1-hydroxyethyl)-2-methylbenzene-1-sulfonamide

생성물 1

HCID 2169Amosulalol

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매HCID 178418361HCID 178418361, 화합물용매

실험 절차

In 200 ml of methanol was dissolved 20 g of 5-{1-hydroxy-2-[N-benzyl-2-(2-methoxyphenoxy)ethylamino]ethyl}-2-methylbenzenesulfonamide. After adding thereto 20 ml of ethanol containing about 10% hydrogen chloride and 1 g of 10% palladium charcoal, the mixture was shaked in hydrogen gas stream. When the absorption of hydrogen stopped, the catalyst was filtered away and the filtrate was distilled off under reduced pressure. The residue was dissolved in 100 ml of ethanol while it was hot and the solution was allowed to stand overnight in ice chamber, whereby 12.8 g of the α-type crystals of 5-{1-hydroxy-2-[2-(2-methoxyphenoxy)ethylamino]-ethyl}-2-methylbenzenesulfonamide were obtained as the colorless crystals. The physical and chemical properties of the product were as follows:

후처리

  1. additionAfter adding
  2. customWhen the absorption of hydrogen
  3. filtrationthe catalyst was filtered away
  4. distillationthe filtrate was distilled off under reduced pressure
  5. dissolutionThe residue was dissolved in 100 ml of ethanol while it

출처 및 근거

ORD 기록
ord-43d754f7cda44e6aac8a7c2969dc6aa6
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04217305

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