Triethylamine → Ethyl (2Z)-2-((2,6-dichloropyridin-3-yl)carbonyl)-3-(dimethylamino)prop-2-enoate

HRID 1696934ノート

反応式

HRID 1696934 の反応式
[Cl:1][C:2]1[N:10]=[C:9]([Cl:11])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].CN[C:14]([NH:21][CH3:22])=[CH:15][C:16]([O:18][CH2:19][CH3:20])=[O:17].[CH2:23](N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:3]([C:4](/[C:15](=[CH:14]/[N:21]([CH3:22])[CH3:23])/[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[O:5])=[CH:7][CH:8]=[C:9]([Cl:11])[N:10]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 122639842,6-Dichlorpyridine-3-carbonyl chlorideHCID 85819813Ethyl 3,3-dimethylaminoacrylate

生成物 1

HCID 15675736Ethyl (2Z)-2-((2,6-dichloropyridin-3-yl)carbonyl)-3-(dimethylamino)prop-2-enoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 2,6-dichloronicotinoyl chloride (62.5 g), ethyl 3,3-dimethylaminoacrylate (58.8 g) and triethylamine (69 g) in toluene (600 mL) was stirred at 90° C. for 1 hour then cooled and concentrated. The concentrate was dissolved in dichloromethane (60 mL), diluted with diethyl ether, and filtered. The filtrate was concentrated, and the concentrate was crystallized from dichloromethane/diethyl ether/hexanes.

後処理

  1. temperaturethen cooled
  2. concentrationconcentrated
  3. dissolutionThe concentrate was dissolved in dichloromethane (60 mL)
  4. additiondiluted with diethyl ether
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. customthe concentrate was crystallized from dichloromethane/diethyl ether/hexanes

出典と根拠

ORDレコード
ord-59468fef94ac434f8f11f2f60a94b9e2
出典データセット
uspto-grants-2012_04
特許番号
US08163769B2

反応ノート

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