Ammonia → HCID 58739057, 화합물

HRID 720290노트

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HRID 720290 반응식
[NH3:1].[CH2:2]([O:4][C:5]([C:7]1[N:8]=[C:9](S(C)(=O)=O)[N:10]([CH3:22])[C:11](=[O:21])[C:12]=1[O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:6])[CH3:3]>C(#N)C>[CH2:2]([O:4][C:5]([C:7]1[N:8]=[C:9]([NH2:1])[N:10]([CH3:22])[C:11](=[O:21])[C:12]=1[O:13][CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[O:6])[CH3:3]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 21060065HCID 21060065, 화합물

생성물 1

HCID 58739057HCID 58739057, 화합물수율 59%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Gaseous ammonia was bubbled at 25° C. in a solution of 2-methanesulfonyl-5-benzyloxy-1-methyl-6-oxo-1,6-dihydro-pyrimidine-4-carboxylic acid ethyl ester (0.200 g, 0.55 mmol) in acetonitrile (4 ml). After 30 min, the solvent was evaporated in vacuo and the residue was chromatographed on silica gel (elution toluene-ethyl acetate, 6:4 to 1:1) to give 0.099 g (59% yield) of the title ester as a white solid. 1HNMR 400 MHz (DMSO-d6) δ (ppm): 1.19 (3H, t, J=7.1 Hz, CH3), 3.29 (3H, s, NCH3), 4.18 (2H, q, J=7.1 Hz, OCH2), 4.89 (2H, s, OCH2), 7.21 (2H, broad s, NH2), 7.31–7.37 (5H, m, aromatics). Anal. Calcd for C15H17N3O4: C 59.39; H, 5.64; N, 13.85. Found: C, 59.31; H, 5.46, N 13.72.

후처리

  1. customthe solvent was evaporated in vacuo
  2. customthe residue was chromatographed on silica gel (elution toluene-ethyl acetate, 6:4 to 1:1)

출처 및 근거

ORD 기록
ord-b27fa165f43f4a9da73cc257e745e0a0
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135467B2

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