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Methanol → 3-(4-Methoxybenzylamino)-4-hydroxy-alpha-(tert-butylaminomethyl)benzyl alcohol hydrochloride

HRID 616212
ノート
印刷プレビュー

反応式

HRID 616212 の反応式
[ClH:1].[NH2:2][C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][C:16]=1[OH:17])[CH:6]([OH:13])[CH2:7][NH:8][C:9]([CH3:12])([CH3:11])[CH3:10].[CH3:18][O:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=O)=[CH:22][CH:21]=1.CO>O=[Pt]=O.O>[ClH:1].[CH3:18][O:19][C:20]1[CH:27]=[CH:26][C:23]([CH2:24][NH:2][C:3]2[CH:4]=[C:5]([CH:14]=[CH:15][C:16]=2[OH:17])[CH:6]([OH:13])[CH2:7][NH:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:22][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 312444-MethoxybenzaldehydeHCID 13416921HCID 13416921、化合物

生成物 1

HCID 1629243-(4-Methoxybenzylamino)-4-hydroxy-alpha-(tert-butylaminomethyl)benzyl alcohol hydrochloride

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 962Water溶媒

実験手順

A mixture of 3-amino-4-hydroxy-α-(tert.butylaminomethyl)-benzylalcohol hydrochloride (6.53 g, 0.025 mole), p-methoxybenzaldehyde (3.4 g, 0.025 mole), PtO2 (180 mg), and methanol (125 ml) was placed in a hydrogenation apparatus and hydrogenated at normal pressure (20 - 30 cm H2O superatmospheric) for one hour and 50 minutes. During this period of time, the calculated amount of hydrogen was absorbed, and the hydrogenation was interrupted by supplying argon. The platinum catalyst was filtered off with continued supply of argon, but in spite of this, the filtrate quickly became dark due to oxidation. The filtrate was immediately evaporated in vacuum at 40° - 50° C. The residue which was a light brown foam (9.53 g), was recrystallized twice by precipitation from ethanol/ether (1:1). The yield of the analytical pure 3-(4-methoxybenzylamino)-4-hydroxy-α-(tert.butylaminomethyl)benzylalcohol hydrochloride was 5.2 g (55%), m.p. 196.6° - 197.8° C.

後処理

  1. waitDuring this period of time
  2. customthe calculated amount of hydrogen was absorbed
  3. filtrationThe platinum catalyst was filtered off with continued supply of argon
  4. customThe filtrate was immediately evaporated in vacuum at 40° - 50° C
  5. customwas recrystallized twice by precipitation from ethanol/ether (1:1)

出典と根拠

ORDレコード
ord-90df2bbbc53547ccb0f9b0244b9ec91a
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04072760

反応ノート

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