Ammonia → HCID 58739057、化合物

HRID 720290ノート

反応式

HRID 720290 の反応式
[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]

参加物

4

反応物 2

HCID 222AmmoniaHCID 21060065HCID 21060065、化合物

生成物 1

HCID 58739057HCID 58739057、化合物収率 59%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b27fa165f43f4a9da73cc257e745e0a0
出典データセット
uspto-grants-2006_11
特許番号
US07135467B2

反応ノート

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