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

HRID 907360

반응식

HRID 907360 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2e5dd268b48c466691af1a22b839d19f
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012967B2

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