Hydrochloric Acid → HCID 69655664, 화합물

HRID 11726

반응식

HRID 11726 반응식
[O-]CC.[Na+].[Cl:5][C:6]1[CH:31]=[CH:30][C:9]([O:10][CH2:11][C:12]([N:14]2[CH2:19][C@H:18]([CH3:20])[N:17]([CH2:21][C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[CH2:16][C@H:15]2[CH3:29])=[O:13])=[C:8]([C:32]2[O:36][N:35]=[CH:34][CH:33]=2)[CH:7]=1.Cl.O>C(O)C>[Cl:5][C:6]1[CH:31]=[CH:30][C:9]([O:10][CH2:11][C:12]([N:14]2[CH2:19][C@H:18]([CH3:20])[N:17]([CH2:21][C:22]3[CH:23]=[CH:24][C:25]([F:28])=[CH:26][CH:27]=3)[CH2:16][C@H:15]2[CH3:29])=[O:13])=[C:8]([C:32](=[O:36])[CH2:33][C:34]#[N:35])[CH:7]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 2723922Sodium ethoxideHCID 696553762-(4-Chloro-2-isoxazol-5-yl-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone

생성물 1

HCID 69655664HCID 69655664, 화합물수율 74.2%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To a stirred mixture of sodium ethoxide (0.14 g, 1.0 mmol) in ethanol (2 mL) was added 2-(4-chloro-2-isoxazol-5-yl-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.465 g, 1.0 mmol) in ethanol (3 mL). The resulting mixture was stirred at ambient temperature for 3 hours. To the reaction was then added 3M hydrochloric acid (2 mL) and the resulting solution was poured into water (30 mL). This was extracted with ethyl acetate and the organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. Flash chromatography on silica gel gave the title compound (0.34 g).

후처리

  1. extractionThis was extracted with ethyl acetate
  2. washthe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b0d5cee49b2a4e9c90b66e67686ca1e3
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098212B2

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