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

HRID 1942227

반응식

HRID 1942227 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 3652203-Aminoadamantane-1-carboxylic acid hydrochloride수율 78%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
95 °C

실험 절차

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 (m, 6H), 1.69-1.48 (m, 4H).

후처리

  1. customTo a 3-neck 5 L, flask equipped with a reflux condenser, a mechanical stirrer
  2. customDuring this time, solid material precipitated from the solution
  3. temperatureAfter cooling at 0° C.
  4. filtrationthe solids were filtered
  5. washwashed with acetone
  6. customThe solid was then dried under high vacuum at 50° C. for about 2 hours

출처 및 근거

ORD 기록
ord-1f3a5389c2c74a3d8ca6acc8a87855fd
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389519B2

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