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Water → Ammonia

HRID 1433307
ノート
印刷プレビュー

反応式

HRID 1433307 の反応式
[Si]([O:8][C@H:9]([C:48]1[CH:53]=[CH:52][C:51]([OH:54])=[C:50]([CH2:55][OH:56])[CH:49]=1)[CH2:10][NH:11][CH2:12][CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][C:25]2[CH:30]=[CH:29][C:28]([OH:31])=[C:27]([C@@H:32]([C:42]3[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=3)[CH2:33][CH2:34][N:35]([CH:39]([CH3:41])[CH3:40])[CH:36]([CH3:38])[CH3:37])[CH:26]=2)=[CH:16][CH:15]=1)(C(C)(C)C)(C)C.O.[F-].[NH4+]>CO>[NH3:11].[CH:39]([N:35]([CH:36]([CH3:38])[CH3:37])[CH2:34][CH2:33][C@@H:32]([C:27]1[CH:26]=[C:25]([CH2:24][CH2:23][CH2:22][CH2:21][O:20][C:17]2[CH:16]=[CH:15][C:14]([CH2:13][CH2:12][NH:11][CH2:10][C@H:9]([OH:8])[C:48]3[CH:53]=[CH:52][C:51]([OH:54])=[C:50]([CH2:55][OH:56])[CH:49]=3)=[CH:19][CH:18]=2)[CH:30]=[CH:29][C:28]=1[OH:31])[C:42]1[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1)([CH3:41])[CH3:40]
参加物反応条件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 962WaterHCID 25516Ammonium fluorideHCID 579332274-[(1R)-1-{[tert-butyl(dimethyl)silyl]oxy}-2-({2-[4-(4-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}butoxy)phenyl]ethyl}amino)ethyl]-2-(hydroxymethyl)phenol

生成物 2

HCID 222AmmoniaHCID 248765642-((R)-3-(diisopropylamino)-1-phenylpropyl)-4-(4-(4-(2-((R)-2-hydroxy-2-(4-hydroxy-3-(hydroxymethyl)phenyl)ethylamino)ethyl)phenoxy)butyl)phenol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

4-[(1R)-1-{[tert-butyl(dimethyl)silyl]oxy}-2-({2-[4-(4-{3-[(1R)-3-(diisopropylamino)-1-phenylpropyl]-4-hydroxyphenyl}butoxy)phenyl]ethyl}amino)ethyl]-2-(hydroxymethyl)phenol (Preparation 63, 311 mg, 0.356 mmol) was dissolved in methanol (4 ml) and water (0.5 ml) and ammonium fluoride (132 mg, 3.56 mmol) was added. The reaction was heated to 40° C. and stirred overnight. Reaction mixture was cooled and solvent removed in vacuo. The residue was purified by column chromatography on silica gel eluting with dichloromethane:methanol:880 ammonia (100/0/0 to 90/10/1.0 by volume) to furnish the title compound as a glass, 84 mg.

後処理

  1. customReaction mixture
  2. temperaturewas cooled
  3. customsolvent removed in vacuo
  4. customThe residue was purified by column chromatography on silica gel eluting with dichloromethane

出典と根拠

ORDレコード
ord-f482fe72229e48f683164588595ac071
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07612084B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート