Ethanol → Amosulalol

HRID 1855960ノート

反応式

HRID 1855960 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

HCID 2169Amosulalol

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-43d754f7cda44e6aac8a7c2969dc6aa6
出典データセット
uspto-grants-1980_08
特許番号
US04217305

反応ノート

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