Hydrochloric Acid → 3-Aminoadamantane-1-carboxylic acid hydrochloride

HRID 550859

反応式

HRID 550859 の反応式
C([NH:4][C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][C:7]([C:15]([OH:17])=[O:16])([CH2:8]3)[CH2:6]1)[CH2:12]2)(=O)C.[ClH:18]>O>[ClH:18].[NH2:4][C:5]12[CH2:14][CH:9]3[CH2:10][CH:11]([CH2:13][C:7]([C:15]([OH:17])=[O:16])([CH2:8]3)[CH2:6]1)[CH2:12]2

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 27697143-Acetylamino-adamantane-1-carboxylic acid

生成物 1

HCID 3652203-Aminoadamantane-1-carboxylic acid hydrochloride収率 78%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
95 °C

実験手順

To a 3-neck 5-L flask equipped with a reflux condenser, a mechanical stirrer and a temperature probe was added 3-acetylamino-adamantane-1-carboxylic acid (432 g, 1.82 mol), water (1.00 L) and concentrated hydrochloric acid (2.44 L), and the resulting mixture was heated at 95° C. for 6 days. During this time, solid material precipitated from the solution. After cooling at 0° C., the solids were filtered and washed with acetone. The solid was then dried under high vacuum at 50° C. for about 2 hours to afford 328 g (78%) of the title compound, 3-amino-adamantane-1-carboxylic acid hydrochloride, as a white solid. 1H NMR (300 MHz, DMSO-d6) δ 12.35 (br s, 1H), 8.27 (br s, 3H), 2.22-2.12 (m, 2H), 1.92-1.85 (m, 2H), 1.83-1.71 (ml 6H), 1.69-1.48 (m, 4H).

後処理

  1. customDuring this time, solid material precipitated from the solution
  2. temperatureAfter cooling at 0° C.
  3. filtrationthe solids were filtered
  4. washwashed with acetone
  5. customThe solid was then dried under high vacuum at 50° C. for about 2 hours

出典と根拠

ORDレコード
ord-2776720966dc43d59b8b611d4a1a3ae8
出典データセット
uspto-grants-2011_05
特許番号
US07947680B2

関連ノート

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