HCID 11780885, 화합물 → HCID 131721277, 화합물

HRID 1415706노트

반응식

HRID 1415706 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])[C:4](=[O:20])[CH2:3]1.[C:21]([C@:29]([C:44]([OH:46])=[O:45])([OH:43])[C@:30]([C:35](=[O:42])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)([OH:34])[C:31]([OH:33])=[O:32])(=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>CO>[C:35]([C@:30]([C:31]([OH:33])=[O:32])([OH:34])[C@:29]([C:21](=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([OH:43])[C:44]([OH:46])=[O:45])(=[O:42])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1.[CH3:1][N:2]1[CH2:7][CH2:6][C@H:5]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])[C:4](=[O:20])[CH2:3]1

참가 물질

4

반응물 2

HCID 11780885HCID 11780885, 화합물HCID 12362977Di-benzoyl-d-tartaric acid

생성물 1

HCID 131721277HCID 131721277, 화합물수율 72.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of (±)-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-piperidinone (1.60 g, 5.73 mmoles) and dibenzoyl-D-tartaric acid (2.28 g, 315 mmol) in 10 mL of methanol was heated at reflux temperature under argon atmosphere and it was cooled to room temperature. After stirring overnight at room temperature the precipitated solid was filtered, washed with a small amount of methanol to obtain the first crop of (R)-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-piperidinone dibenzoyl-D-tartaric acid salt (2.65 g). The filtrate solution was concentrated to a volume of ca 6 mL and was stirred at ambient temperature for one day. The second crop of the chiral salt (0.24 g) was obtained by filtering the solid and washed it with a small amount of methanol.

후처리

  1. temperaturewas heated
  2. temperatureat reflux temperature under argon atmosphere
  3. filtrationwas filtered
  4. washwashed with a small amount of methanol

출처 및 근거

ORD 기록
ord-9445d843b76f42ad8bfa7780195a4b8f
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05908934

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