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Water → HCID 178431816, 화합물

HRID 1582225
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HRID 1582225 반응식
C[O-].[Na+].Cl.[NH2:5][C:6]([NH2:8])=[NH:7].N1C=CC=CC=1.[S:15]([OH:35])([O:18][C:19]1[C:20]([CH3:34])=[C:21]2[C:25](=[CH:26][CH:27]=1)[N:24]([CH3:28])[C:23]([C:29](OCC)=[O:30])=[CH:22]2)(=[O:17])=[O:16].O>CN(C)C=O>[S:15]([OH:35])([O:18][C:19]1[C:20]([CH3:34])=[C:21]2[C:25](=[CH:26][CH:27]=1)[N:24]([CH3:28])[C:23]([C:29]([NH:7][C:6]([NH2:8])=[NH:5])=[O:30])=[CH:22]2)(=[O:16])=[O:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 5742Guanidine HydrochlorideHCID 10942334Sodium MethoxideHCID 22719997HCID 22719997, 화합물

생성물 1

HCID 178431816HCID 178431816, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of sodium methoxide (4.28 g, 79.2 mmol), guanidine hydrochloride (7.58 g, 79.3 mmol) and N,N-dimethylformamide (70 ml) was stirred at room temperature for 1 hour, and then the insoluble material was filtered off. A solution of 2-ethoxycarbonyl-1,4-dimethyl-1H-indole-5-yl hydrogen sulfate pyridine salt (3.11 g, 7.92 mmol) in N,N-dimethylformamide (10 ml) was added to the filtrate, and the resulting mixture was stirred at room temperature for 7.5 hours. Water was added to the reaction mixture, followed by washing with chloroform. Subsequently, chloroform and then 2N hydrochloric acid were added and the solid thus precipitated was collected by filtration and washed with methanol to obtain 2.12 g of 2-[[[amino(imino)-methyl]amino]carbonyl]-1,4-dimethyl-1H-indol-5-yl hydrogen sulfate.

후처리

  1. filtrationthe insoluble material was filtered off
  2. stirringthe resulting mixture was stirred at room temperature for 7.5 hours
  3. washby washing with chloroform
  4. additionSubsequently, chloroform and then 2N hydrochloric acid were added
  5. customthe solid thus precipitated
  6. filtrationwas collected by filtration
  7. washwashed with methanol

출처 및 근거

ORD 기록
ord-037b4ad781624dda99ca11115e5c1d23
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06734205B2

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