Dicyclohexylcarbodiimide → Manidipine

HRID 1475169

反応式

HRID 1475169 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)[C:9]([C:20]([OH:22])=[O:21])=[C:8]([CH3:23])[NH:7][C:6]=1[CH3:24])=[O:4].C1(N=C=NC2CCCCC2)CCCCC1.CN(C1C=CC=CN=1)C.[CH:49]([N:62]1[CH2:67][CH2:66][N:65]([CH2:68][CH2:69]O)[CH2:64][CH2:63]1)([C:56]1[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1)[C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1>C1(C)C=CC=CC=1>[CH3:24][C:6]1[NH:7][C:8]([CH3:23])=[C:9]([C:20]([O:22][CH2:69][CH2:68][N:65]2[CH2:64][CH2:63][N:62]([CH:49]([C:56]3[CH:57]=[CH:58][CH:59]=[CH:60][CH:61]=3)[C:50]3[CH:51]=[CH:52][CH:53]=[CH:54][CH:55]=3)[CH2:67][CH2:66]2)=[O:21])[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)[C:5]=1[C:3]([O:2][CH3:1])=[O:4]

参加物

6

反応物 4

HCID 10868DicyclohexylcarbodiimideHCID 218852-DimethylaminopyridineHCID 1733222,6-Dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylic acid monomethyl esterHCID 47425734-(Diphenylmethyl)-1-piperazineethanol

生成物 1

HCID 4008Manidipine収率 54.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
72.5 °C

実験手順

To a suspension of 2,6-dimethyl-4-(3-nitro-phenyl)-1,4-dihydro-pyridine-3,5-dicarboxylic acid monomethyl ester (5 gm), dicyclohexyl carbodiimide (3.08 gm) and dimethylamino pyridine (0.25 gm) in toluene (30 ml) at room temperature was added 2-(4-benzhydryl piperazine-1-yl)ethanol (7.5 gm). Reaction mass was then heated to 70-75° C. for 2 hours. Reaction mass was then cooled to room temperature and filtered. Toluene layer was concentrated under vacuum to get manidipine base (5 gm).

後処理

  1. customReaction mass
  2. customReaction mass
  3. temperaturewas then cooled to room temperature
  4. filtrationfiltered
  5. concentrationToluene layer was concentrated under vacuum

出典と根拠

ORDレコード
ord-560eb7a71ae64a37af1fd5388192132e
出典データセット
uspto-grants-2015_04
特許番号
US09018376B2

関連ノート

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