Acetic Acid → (2s)-Benzhydryl-3-quinuclidinone l-tartaric acid salt

HRID 982872

반응식

HRID 982872 반응식
[CH:1]([CH:14]1[C:19](=[O:20])[CH:18]2[CH2:21][CH2:22][N:15]1[CH2:16][CH2:17]2)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(O)(=O)C.[C:27]([OH:36])(=[O:35])[C@@H:28]([C@H:30]([C:32]([OH:34])=[O:33])[OH:31])[OH:29]>C(O)C>[C:27]([OH:36])(=[O:35])[C@@H:28]([C@H:30]([C:32]([OH:34])=[O:33])[OH:31])[OH:29].[CH:1]([C@H:14]1[C:19](=[O:20])[CH:18]2[CH2:17][CH2:16][N:15]1[CH2:22][CH2:21]2)([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 4251102-Benzhydryl-3-quinuclidinoneHCID 444305L-Tartaric acid

생성물 1

HCID 131724767(2s)-Benzhydryl-3-quinuclidinone l-tartaric acid salt

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Racemic 2-benzhydryl-3-quinuclidinone (52.45 g, 180 mmol) was dissolved in denatured ethanol (525 ml) with acetic acid (10.4 ml, 180 mmol) and L-tartaric acid (27 g, 180 mmol) was added. The mixture was heated to reflux for 12 hours and then allowed to cool to room temperature and held for one hour. The solids were collected and dried under vacuum at 40° C. for 12 hours. The yield of the desired salt was 69.9 g, 88% of theory.

후처리

  1. additionwas added
  2. temperatureThe mixture was heated
  3. temperatureto reflux for 12 hours
  4. customThe solids were collected
  5. customdried under vacuum at 40° C. for 12 hours

출처 및 근거

ORD 기록
ord-395763701c28443a87cf1c2ec3dbf351
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06861526B2

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