Oxalic Acid → HCID 9837977, 화합물

HRID 1655102노트

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HRID 1655102 반응식
[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

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 15186066HCID 15186066, 화합물

생성물 1

HCID 9837977HCID 9837977, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-31aa152bd6c544f7a48204873742d315
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05409946

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