1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 2-chloro-6-methyl-N-(1-methyl-1-phenylethyl)nicotinamide

HRID 21343ノート

反応式

HRID 21343 の反応式
[Cl:1][C:2]1[N:10]=[CH:9][C:8](C)=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH3:12]CN=C=NCCCN(C)C.C1C=C2N=NN(O)C2=CC=1.O.[C:34]([NH2:43])([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)([CH3:36])[CH3:35]>CN(C=O)C.O>[Cl:1][C:2]1[N:10]=[C:9]([CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([NH:43][C:34]([CH3:36])([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[CH3:35])=[O:6]

参加物

7

反応物 4

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 68509CumylamineHCID 27960291-Hydroxybenzotriazole hydrateHCID 123877302-Chloro-5-methylnicotinic acid

生成物 1

HCID 866283402-chloro-6-methyl-N-(1-methyl-1-phenylethyl)nicotinamide収率 62%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

In a similar manner to Step 1 of Example 137, 2-chloro-5-methylnicotinic acid (2.00 g, 11.7 mmol) was dissolved in DMF (40 mL), and the solution was treated with EDCI (3.35 g, 17.5 mmol), HOBT monohydrate (890 mg, 5.83 mmol) and cumylamine (3.40 mL, 23.3 mmol). The mixture was added with water. The precipitated solid was collected by filtration and dried under reduced pressure to obtain 2-chloro-6-methyl-N-(1-methyl-1-phenylethyl)nicotinamide (2.09 mg, yield 62%).

後処理

  1. filtrationThe precipitated solid was collected by filtration
  2. customdried under reduced pressure

出典と根拠

ORDレコード
ord-9127249f319244ed9a3d3dc663bb9562
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

反応ノート

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