HCID 11780885、化合物 → HCID 131721277、化合物

HRID 1415706ノート

反応式

HRID 1415706 の反応式
[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

参加物

4

反応物 2

HCID 11780885HCID 11780885、化合物HCID 12362977Di-benzoyl-d-tartaric acid

生成物 1

HCID 131721277HCID 131721277、化合物収率 72.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9445d843b76f42ad8bfa7780195a4b8f
出典データセット
uspto-grants-1999_06
特許番号
US05908934

反応ノート

読み込み中…