Oxalic Acid → HCID 9837977、化合物

HRID 1655102ノート

反応式

HRID 1655102 の反応式
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][C:8]1[CH:12]=[C:11]([CH:13]2[CH2:17][CH2:16][CH2:15][N:14]2[CH3:18])[O:10][N:9]=1>C(OCC)C>[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][C:8]1[CH:12]=[C:11]([C@@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[CH3:18])[O:10][N:9]=1

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 15186066HCID 15186066、化合物

生成物 1

HCID 9837977HCID 9837977、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of oxalic acid (51 mg, 0.57 mmol) in diethyl ether was added dropwise to a stirring solution of 3-methyl-5-(1-methyl-2-pyrrolidinyl)-isoxazole (62.8 mg, 0.38 mmol), from Example 2a, in diethyl ether. After 0.5 hour of stirring at ambient temperature, the reaction flask became coated with a glass-like clear colorless solid. The diethyl ether was evaporated and the solid was triturated several times with diethyl ether to give, after evaporation of the solvent in vacuo, 102 mg of the title compound (2b). MS (DCl/NH3) m/e 167 (M+H)+, 184 (M+NH4)+. 1H NMR (D2O) δ: 2.11-2.33 (m, 3H), 2.31 (s, 3H), 2.49-2.60 (m, 1H), 2.48 (dd, 2H), 4.92 (t, 1H), 6.52 (s, 1H). Anal. calcd. for C10H13NO5.0.2H2O.0.2C2H2O 2 : C, 48.65; H, 6.16; N, 9.95. Found: C, 48.80; H, 5.90; N, 9.77.

後処理

  1. customThe diethyl ether was evaporated
  2. customthe solid was triturated several times with diethyl ether
  3. customto give
  4. customafter evaporation of the solvent in vacuo, 102 mg of the title compound (2b)

出典と根拠

ORDレコード
ord-31aa152bd6c544f7a48204873742d315
出典データセット
uspto-grants-1995_04
特許番号
US05409946

反応ノート

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