Hydrochloric Acid → 1-((6-chloropyridin-3-yl)methyl)-2,3,5,6,7,8-hexahydro-1H-5,8-epoxyimidazo[1,2-a]azepine-9-carbonitrile

HRID 1043523ノート

反応式

HRID 1043523 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]2[CH2:13][CH2:12][NH:11][C:10]2=[CH:14][C:15]#[N:16])=[CH:4][CH:3]=1.[CH:17](=[O:22])[CH2:18][CH2:19][CH:20]=O.Cl>C(#N)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:9]2[C:10]3=[C:14]([C:15]#[N:16])[CH:20]4[O:22][CH:17]([N:11]3[CH2:12][CH2:13]2)[CH2:18][CH2:19]4)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 12524ButanedialHCID 743284342-(1-((6-Chloropyridin-3-yl)methyl)imidazolidin-2-ylidene)acetonitrile

生成物 1

HCID 866589441-((6-chloropyridin-3-yl)methyl)-2,3,5,6,7,8-hexahydro-1H-5,8-epoxyimidazo[1,2-a]azepine-9-carbonitrile収率 66%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a 50 ml round bottom flask was added 1.17 g (0.005 mol) 2-(1-((6-chloropyridin-3-yl)methyl)imidazolidin-2-ylidene)acetonitrile, 30 ml dry acetonitrile and 0.860 g (0.01 mol) succinaldehyde and catalytic concentrated HCl. The reaction was stirred at r.t. and monitored by TLC. After completion, the mixture was evaporated to remove solvent and purified by column chromatography to afford final product as faint yellow powder with 66% yield.

後処理

  1. customAfter completion, the mixture was evaporated
  2. customto remove solvent
  3. custompurified by column chromatography

出典と根拠

ORDレコード
ord-7129a57a4f2f46cd8d13d886b35a99f9
出典データセット
uspto-grants-2013_10
特許番号
US08563546B2

反応ノート

読み込み中…