Dimethylformamide → HCID 9951306, 화합물

HRID 1265043노트

반응식

HRID 1265043 반응식
[O:1]=[C:2]1[NH:6][C:5](=[O:7])[CH:4]([CH2:8][C:9]2[CH:10]=[CH:11][C:12]([O:18][CH3:19])=[C:13]([CH:17]=2)[C:14]([OH:16])=O)[S:3]1.[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][NH2:27].Cl.CN(C)CCCN=C=NCC.CN(C)C=O>O>[N:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][NH:27][C:14](=[O:16])[C:13]1[CH:17]=[C:9]([CH2:8][CH:4]2[S:3][C:2](=[O:1])[NH:6][C:5]2=[O:7])[CH:10]=[CH:11][C:12]=1[O:18][CH3:19]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 195092-PyridinemethanamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 9943613HCID 9943613, 화합물

생성물 1

HCID 9951306HCID 9951306, 화합물수율 20%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5-[(2,4-Dioxothiazolidin-5-yl)methyl]-2-methoxybenzoic acid (282 mg, 1.00 mmol), 2-picolylamine (114 mg, 1.05 mmol), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (230 mg, 1.20 mmol) and N,N-dimethylformamide (5 mL) were mixed and stirred for 5.5 hours at room temperature, which was then allowed to stand overnight. After water was added to the reaction mixture, this was made acidic and extracted with ethyl acetate. The extracted solution was dried and then concentrated. The residue was recrystallized from acetonitrile to obtain 73.7 mg (20%) of the title compound as colorless crystals.

후처리

  1. waitto stand overnight
  2. extractionextracted with ethyl acetate
  3. customThe extracted solution was dried
  4. concentrationconcentrated
  5. customThe residue was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-beea16d6ea6d467d8c4e3251ca736dc0
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06545026B1

반응 노트

불러오는 중…