Metoprolol → (S)-Metoprolol

HRID 1087281

反応式

HRID 1087281 の反応式
[CH3:1][CH:2]([NH:4][CH2:5][CH:6]([OH:19])[CH2:7][O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][O:17][CH3:18])=[CH:13][CH:14]=1)[CH3:3].C(O)(=O)/C=C/C=C/C>CC(C)=O>[CH3:3][CH:2]([NH:4][CH2:5][C@H:6]([OH:19])[CH2:7][O:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][CH2:16][O:17][CH3:18])=[CH:13][CH:14]=1)[CH3:1]

参加物

4

反応物 2

HCID 4171MetoprololHCID 643460Sorbic Acid

生成物 1

HCID 157716(S)-Metoprolol収率 115.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
0 °C

実験手順

To the stirred acetone solution of metoprolol base (19.3 mol), acetone (30 l) and sorbic acid (2.12 kg, 18.9 mol) were added at room temperature. The mixture was heated to reflux and the hot solution was filtered. The filtrate was allowed to cool slowly to 0° C. The crystals were centrifugated off, washed with cold acetone (10 l) and dried for three days in vacuo at room temperature to yield 5.95 kg of crystalline (S)-metoprolol. (81% from (4)).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. filtrationthe hot solution was filtered
  4. washwashed with cold acetone (10 l)
  5. customdried for three days in vacuo at room temperature

出典と根拠

ORDレコード
ord-ecc3204946d546b58f26672c8d79018c
出典データセット
uspto-grants-1991_07
特許番号
US05034535

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