홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrochloric Acid → N'-(1-benzyl-4-methyl-5-nitro-6-oxopyrimidin-2-yl)-N,N-dimethylmethanimidamide

HRID 1516833
노트
인쇄 미리보기

반응식

HRID 1516833 반응식
[CH3:1][N:2]([CH3:16])/[CH:3]=[N:4]/[C:5]1[NH:6][C:7](=[O:15])[C:8]([N+:12]([O-:14])=[O:13])=[C:9]([CH3:11])[N:10]=1.C1CCN2C(=NCCC2)CC1.[CH2:28](Br)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.Cl>CN(C=O)C>[CH2:28]([N:6]1[C:7](=[O:15])[C:8]([N+:12]([O-:14])=[O:13])=[C:9]([CH3:11])[N:10]=[C:5]1/[N:4]=[CH:3]/[N:2]([CH3:1])[CH3:16])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene2회HCID 1355361192-[(Dimethylamino)methylene]amino-6-methyl-5-nitro-4-pyrimidinol

생성물 1

HCID 11186127N'-(1-benzyl-4-methyl-5-nitro-6-oxopyrimidin-2-yl)-N,N-dimethylmethanimidamide수율 85,493.203%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of (E)-N,N-Dimethyl-N′-(4-methyl-5-nitro-6-oxo-1,6-dihydropyrimidin-2-yl)formimidamide (53.4 g, 0.24 mmol) in DMF (690 mL) was added DBU (44.6 mL, 0.30 mol) and benzyl bromide (44.4 mL, 0.29 mol) and stirred at room temperature for 1 h. The excess of DBU was neutralized with HCl, and the mixture was concentrated in vacuo. The residue was dissolved in methylene chloride and extracted twice with 2M HCl and water, then dried over Na2SO4 and concentrated. Trituration with ethanol afforded the crystalline product which was washed with ethanol to give the product (64.7 g, 86% yield) and used in the next step without further purification.

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. dissolutionThe residue was dissolved in methylene chloride
  3. extractionextracted twice with 2M HCl and water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customTrituration with ethanol afforded the crystalline product which
  7. washwas washed with ethanol

출처 및 근거

ORD 기록
ord-7c64de0dd6be42b994556cd9606e58ab
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08227601B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트