Flordipine → 1,4-Dihydro-2,6-dimethyl-1-[2-(4-morpholinyl)ethyl]-4-[2-(trifluoromethyl)phenyl]-3,5-pyridinedicarboxylate maleate

HRID 2164320

反応式

HRID 2164320 の反応式
[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:9][C:10]1[N:11]([CH2:37][CH2:38][N:39]2[CH2:44][CH2:43][O:42][CH2:41][CH2:40]2)[C:12]([CH3:36])=[C:13]([C:31]([O:33]CC)=[O:32])[CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]([F:30])([F:29])[F:28])[C:15]=1[C:16]([O:18]CC)=[O:17]>CC(C)=O.C1(C)C=CC=CC=1>[C:1]([OH:8])(=[O:7])/[CH:2]=[CH:3]\[C:4]([OH:6])=[O:5].[CH3:36][C:12]1[N:11]([CH2:37][CH2:38][N:39]2[CH2:40][CH2:41][O:42][CH2:43][CH2:44]2)[C:10]([CH3:9])=[C:15]([C:16]([OH:18])=[O:17])[CH:14]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[C:27]([F:30])([F:28])[F:29])[C:13]=1[C:31]([OH:33])=[O:32]

参加物

5

反応物 2

HCID 53699FlordipineHCID 444266Maleic Acid

生成物 1

HCID 704864011,4-Dihydro-2,6-dimethyl-1-[2-(4-morpholinyl)ethyl]-4-[2-(trifluoromethyl)phenyl]-3,5-pyridinedicarboxylate maleate収率 106.9%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 1140Toluene溶媒

実験手順

A solution of 1.2 g (0.010 mol) of maleic acid in 6 ml of acetone was poured into a solution of 5.1 g (0.010 mole) of diethyl 1,4-dihydro-2,6-dimethyl-1-[2-(4-morpholinyl)ethyl]-4-[2-(trifluoromethyl)phenyl]-3,5-pyridinedicarboxylate in 30 ml of toluene. The precipitated solid was collected, washed with toluene, and dried to yield 6.1 g (97%) of 1,4-dihydro-2,6-dimethyl-1-[2-(4-morpholinyl)ethyl]-4-[2-(trifluoromethyl)phenyl]-3,5-pyridinedicarboxylate maleate. This material was partitioned between 30 ml of toluene and 25 ml of 10% aqueous NaOH and the separated toluene phase was diluted with 60 ml of heptane. Chilling overnight yielded 3.4 g (67%) of diethyl 1,4-dihydro-2,6-dimethyl-1-[2-(4-morpholinyl)ethyl[4-[2-(trifluoromethyl)phenyl]-3,5-pyridinedicarboxylate. Recrystallization from 10 ml of 2-propanol yielded 2.9 g of the title compound which contained, as determined by HPLC, 0.19% of ##STR11##

後処理

  1. customThe precipitated solid was collected
  2. washwashed with toluene
  3. customdried

出典と根拠

ORDレコード
ord-1cebbd3f52ea414bae366161a590587d
出典データセット
uspto-grants-1985_03
特許番号
US04503223

関連ノート

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