Dimethylamine → HCID 4467695, 화합물

HRID 1446154노트

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HRID 1446154 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([C:13](O)=[O:14])=[C:11]([CH3:16])[O:10][N:9]=1.S(Cl)(Cl)=O.[CH3:21][NH:22][CH3:23]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([C:13]([N:22]([CH3:23])[CH3:21])=[O:14])=[C:11]([CH3:16])[O:10][N:9]=1

참가 물질

4

반응물 3

HCID 674DimethylamineHCID 24386Thionyl ChlorideHCID 902034-Isoxazolecarboxylic acid, 3-(2-chlorophenyl)-5-methyl-

생성물 1

HCID 4467695HCID 4467695, 화합물수율 23.6%

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온도
60 °C

실험 절차

To 3-(2-chlorophenyl)-5-methylisoxazol-4-carboxylic acid (25 mg, 0.10 mmol) was added thionyl chloride (1 mL) and the neat solution allowed to stir 60° C. After 30 min, excess thionyl chloride was evaporated and dimethyl amine (40 μL, 0.08 mmol, 2M in tetrahydrofuran) was added and allowed to stir overnight at ambient temperature. The residue was purified using reversed phase HPLC to afford the title compound (5 mg). HRMS (ESI, pos. ion) m/z calcd for C13H13ClN2O2: 264.0666, found 264.0669.

후처리

  1. customexcess thionyl chloride was evaporated
  2. stirringto stir overnight at ambient temperature
  3. customThe residue was purified

출처 및 근거

ORD 기록
ord-0d5037ad7476428a856729169b98b565
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666888B2

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