Triethylamine → n-[3-(Dimethylamino)propyl]-1-methyl-4-nitro-1h-pyrrole-2-carboxamide

HRID 907360

反応式

HRID 907360 の反応式
[CH3:1][N:2]1[CH:6]=[C:5]([N+:7]([O-:9])=[O:8])[CH:4]=[C:3]1[C:10](Cl)=[O:11].C[CH:14]([NH:16]P(OC1C=CC(Cl)=CC=1Cl)(OC)=S)C.C[CH2:31][N:32]([CH2:35][CH3:36])[CH2:33]C>C(Cl)Cl>[CH3:31][N:32]([CH3:33])[CH2:35][CH2:36][CH2:14][NH:16][C:10]([C:3]1[N:2]([CH3:1])[CH:6]=[C:5]([N+:7]([O-:9])=[O:8])[CH:4]=1)=[O:11]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9299ZytronHCID 110631851-Methyl-4-nitro-1H-pyrrole-2-carbonyl chloride

生成物 1

HCID 15625149n-[3-(Dimethylamino)propyl]-1-methyl-4-nitro-1h-pyrrole-2-carboxamide収率 74%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 1-methyl-4-nitro-1H-pyrrole-2-carbonyl chloride (0.254 g, 1.35 mmol; see Preparation 1(ii) above) in DCM (10 mL), is added dropwise to a solution of DMPA (0.153 g, 5.05 mmol) (Aldrich), NEt3 (0.152 g, 1.5 mmol), in DCM (10 mL) over 15 min. The resulting solution was allowed to stir overnight, before quenching the reaction with a 5% NaOH solution (20 mL). The DCM fraction was then dried over MgSO4, filtered and the solvent removed under reduced pressure to yield the sub-title compound (0.254 g, 74%).

後処理

  1. custombefore quenching
  2. customthe reaction with a 5% NaOH solution (20 mL)
  3. dry with materialThe DCM fraction was then dried over MgSO4
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-2e5dd268b48c466691af1a22b839d19f
出典データセット
uspto-grants-2011_09
特許番号
US08012967B2

関連ノート

読み込み中…