1,2-Dimethylhydrazine dihydrochloride → HCID 18442536, 화합물

HRID 458688

반응식

HRID 458688 반응식
[CH2:1]([O:8][C:9]1[C:14](=[O:15])[N:13]([CH2:16][C:17]([O:19]C)=O)[C:12](S(C)(=O)=O)=[N:11][C:10]=1[C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.Cl.[CH3:32][NH:33][NH:34][CH3:35].C(N(CC)C(C)C)(C)C>CN(C)C=O>[CH2:1]([O:8][C:9]1[C:14](=[O:15])[N:13]2[C:12]([N:33]([CH3:32])[N:34]([CH3:35])[C:17](=[O:19])[CH2:16]2)=[N:11][C:10]=1[C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 93801,2-Dimethylhydrazine dihydrochlorideHCID 81531DiisopropylethylamineHCID 184425315-Benzyloxy-2-methanesulfonyl-1-methoxycarbonylmethyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester

생성물 1

HCID 18442536HCID 18442536, 화합물수율 69%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
22 °C

실험 절차

A mixture of intermediate 3, ethyl 5-benzyloxy-1-(methoxycarbonylmethyl)-2-(methylsulfonyl)-6-oxo-1,6-dihydropyrimidine-4-carboxylate, (0.487 g, 1.15 mmol) in N,N-dimethylformamide (25 ml) was treated with 1,2-dimethylhydrazine dihydrochloride (1.56 g, 11.7 mmol) followed by N,N-diisopropylethylamine (4.1 ml, 11.7 mmol) and the resulting mixture stirred at 22° C. for 4 h. The solvent was then removed in vacuo and the residue diluted with ethyl acetate, washed successively with saturated sodium bicarbonate and brine then dried over anhydrous magnesium sulfate. Evaporation of the solvent followed by chromatography on silica gel (elution with a gradient of ethyl acetate 0–50% in toluene) gave 0.294 g (69% yield) of the title ester as a clear syrup.

후처리

  1. customThe solvent was then removed in vacuo
  2. additionthe residue diluted with ethyl acetate
  3. washwashed successively with saturated sodium bicarbonate and brine
  4. dry with materialthen dried over anhydrous magnesium sulfate
  5. customEvaporation of the solvent
  6. washelution with a gradient of ethyl acetate 0–50% in toluene)

출처 및 근거

ORD 기록
ord-c4ad857185174b728b2b069bd279f61c
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07192948B2

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