1,1,3,3-Tetramethylguanidine → HCID 178467224, 화합물

HRID 638218노트

반응식

HRID 638218 반응식
Br[C:2](=[CH:6]OCC)[C:3](=[O:5])[CH3:4].Cl.[OH:11][CH2:12][C:13]([NH2:15])=[NH:14].CN(C)C(N(C)C)=N>CC(C)=O>[OH:11][CH2:12][C:13]1[NH:14][CH:6]=[C:2]([C:3](=[O:5])[CH3:4])[N:15]=1

참가 물질

5

반응물 3

HCID 664601,1,3,3-TetramethylguanidineHCID 122173662-Hydroxy-acetamidine hydrochlorideHCID 534237433-Bromo-4-ethoxybut-3-EN-2-one

생성물 1

HCID 178467224HCID 178467224, 화합물수율 21%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

9.7 g (0.05 mole) of 3-bromo-4-ethoxy-3-buten-2-one was combined with 5.53 (0.05 mole) of hydroxyacetamidine hydrochloride in 100 ml acetone to form a slurry. To the slurry at 25° C. was added 11.5 g (0.1 mole) of 1,1,3,3-tetramethylguanidine over a period of 5 minutes. After stirring for 48 hours the slurry was filtered and the mother liquors were concentrated in vacuo to an oil which was chromatographed on silica gel 60 (E. Merck) using chloroform as eluent to give 1.48 g (21%) of 2-hydroxymethyl-4-acetylimidazole, m.p. 147°-148° C. 1H-NMR(DMSO-d6)ppm(delta): 7.73 (s, 1H), 5.46 (very broad s, 1H), 4.5 (broad s, 2H), 2.4 (s, 3H).

후처리

  1. customto form a slurry
  2. filtrationwas filtered
  3. concentrationthe mother liquors were concentrated in vacuo to an oil which
  4. customwas chromatographed on silica gel 60 (E. Merck)

출처 및 근거

ORD 기록
ord-3f27b471bf8346c5b6954c4488b46dc9
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04560690

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