Ammonium Hydroxide → o-Desmethyl metoclopramide

HRID 620246

反応式

HRID 620246 の反応式
[OH-].[NH4+].Cl.[NH2:4][C:5]1[C:20]([Cl:21])=[CH:19][C:8]([C:9]([NH:11][CH2:12][CH2:13][N:14]([CH2:17][CH3:18])[CH2:15][CH3:16])=[O:10])=[C:7]([OH:22])[CH:6]=1>O>[NH2:4][C:5]1[C:20]([Cl:21])=[CH:19][C:8]([C:9]([NH:11][CH2:12][CH2:13][N:14]([CH2:15][CH3:16])[CH2:17][CH3:18])=[O:10])=[C:7]([OH:22])[CH:6]=1

参加物

4

反応物 2

HCID 14923Ammonium HydroxideHCID 141168774-amino-5-chloro-N-(2-(diethylamino)ethyl)-2-hydroxybenzamide hydrochloride

生成物 1

HCID 9817332o-Desmethyl metoclopramide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To stirred concentrated ammonium hydroxide (6 ml) was added 4-amino-5-chloro-N-[2-(diethylamino)ethyl]-2-hydroxybenzamide hydrochloride (3.0 grams, 0.0093 mole) and the mixture stirred an additional five minutes followed by the addition of three to four ml of water and another five minute stirring. After filtration the solid was washed two times with three ml of water each time to give, after drying, 2.37 g of the title compound, mp 134°-136° C. NMR spectrum (90 MHz) in CDCl3 gave the following resonances δ: 7.26 (s, 1H); 6.90 (s, 1H); 6.14 (s, 1H); 4.39 (s, 2H); 3.40 (s, 2H); 2.60 (multiplet, 6H); 1.06 (t, 6H).

後処理

  1. stirringstirring
  2. filtrationAfter filtration the solid
  3. washwas washed two times with three ml of water each time
  4. customto give
  5. customafter drying
  6. customNMR spectrum (90 MHz) in CDCl3 gave the following resonances

出典と根拠

ORDレコード
ord-4f0df26f1e5449f98bd2639c6581b88b
出典データセット
uspto-grants-1989_04
特許番号
US04820715

関連ノート

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