Sodium Hydroxide → HCID 19095406, 화합물

HRID 486517노트

반응식

HRID 486517 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]([CH2:14][CH2:15][NH:16][C:17](=O)[CH3:18])[CH:11]=[CH:12][CH:13]=2)=[CH:5][CH:4]=1.P(Cl)(Cl)(Cl)=O.[OH-].[Na+].[C:27]([OH:34])(=[O:33])/[CH:28]=[CH:29]/[C:30]([OH:32])=[O:31]>O.C(O)C>[C:27]([OH:34])(=[O:33])/[CH:28]=[CH:29]/[C:30]([OH:32])=[O:31].[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:10]3[CH2:14][CH2:15][N:16]=[C:17]([CH3:18])[C:11]3=[CH:12][CH:13]=2)=[CH:5][CH:4]=1

참가 물질

7

반응물 4

HCID 14798Sodium Hydroxide2회HCID 24813Phosphorus oxychlorideHCID 444972Fumaric AcidHCID 19095262N-[2-[2-(4-Methoxyphenyl)-1H-pyrrol-1-yl]ethyl]acetamide

생성물 1

HCID 19095406HCID 19095406, 화합물수율 42%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

N-[2-[2-(p-Methoxyphenyl)-pyrrol-1-yl]ethyl]-acetamide (2.1 g) was treated with 10 ml of phosphorus oxychloride under argon and boiled for 1/2 hour while stirring. The reaction mixture was hydrolyzed at 0° C. with 100 ml of 2N sodium hydroxide solution and 50 ml of 28% sodium hydroxide solution, diluted with 600 ml of water and extracted three times with 100 ml of methylene chloride each time. The organic extracts were combined, dried with MgSO4 and freed from solvent. 1.0 g of a total of 2.0 g of crude product was dissolved in a 40-fold amount of ethanol and treated with 1.1 equivalents of a saturated solution of fumaric acid in ethanol. There was obtained 0.6 g (42%) of 3,4-dihydro-6-(p-methoxyphenyl)-1-methyl-pyrrolo[1,2-a]pyrazine fumarate (1:1); m.pt.: 167°-169° C. (dec.).

후처리

  1. extractionextracted three times with 100 ml of methylene chloride each time
  2. dry with materialdried with MgSO4
  3. dissolution1.0 g of a total of 2.0 g of crude product was dissolved in a 40-fold amount of ethanol

출처 및 근거

ORD 기록
ord-8d1acd49ce3b4d6886cf8fd5984397f2
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292732

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