Potassium Carbonate → HCID 178451398、化合物

HRID 733422ノート

反応式

HRID 733422 の反応式
[C:1]([O:5][C:6]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][CH:11]([CH:16]1[C:29]3[CH:28]=[CH:27][C:26]([C:30]#[N:31])=[CH:25][C:24]=3[O:23][C:22]3[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:12]2)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.NO.C(=O)([O-])[O-].[K+].[K+].Cl.[OH-:42].[NH4+:43]>C(O)C.O>[C:1]([O:5][C:6]([N:8]1[CH:9]2[CH2:15][CH2:14][CH:13]1[CH2:12][CH:11]([CH:16]1[C:29]3[CH:28]=[CH:27][C:26]([C:30](=[NH:43])[NH:31][OH:42])=[CH:25][C:24]=3[O:23][C:22]3[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:10]2)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

7

反応物 4

HCID 11430Potassium Carbonate2 回HCID 443297Hydroxyamine hydrochlorideHCID 13908798HCID 13908798、化合物HCID 578392203-(3-cyano-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester

生成物 1

HCID 178451398HCID 178451398、化合物収率 102%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of 3-(3-cyano-9H-xanthen-9-yl)-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (635 mg; 0.877 mmol) in ethanol (10 mL) was added hydroxylamine hydrochloride (183 mg; 2.62 mmol) and potassium carbonate (242 mg; 1.75 mmol), and the mixture was heated to reflux for 16 h. More ammonium hydroxide hydrochloride (183 mg; 2.62 mmol) and potassium carbonate (242 mg; 1.75 mmol) were added, and the mixture was heated to reflux for 24 h. The mixture was allowed to cool to rt, water was added, and the solid was collected by filtration, yielding 402 mg (quant.) of 3-[3-(N-hydroxycarbamimidoyl)-9H-xanthen-9-yl]-8-aza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester, 1n. The crude material was used as such in the next reaction.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 16 h
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 24 h
  5. filtrationthe solid was collected by filtration

出典と根拠

ORDレコード
ord-46291a43213e42a3af44200c1a6b9079
出典データセット
uspto-grants-2009_09
特許番号
US07589104B2

反応ノート

読み込み中…