Ammonium Chloride → HCID 178519825, 화합물

HRID 1913526노트

반응식

HRID 1913526 반응식
[Si]([O:8][C@H:9]1[CH2:14][CH2:13][C@H:12]([N:15]2[CH:19]=[C:18]([CH:20]=[O:21])[N:17]=[CH:16]2)[CH2:11][CH2:10]1)(C(C)(C)C)(C)C.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Cl-].[NH4+]>O1CCCC1>[OH:8][C@H:9]1[CH2:10][CH2:11][C@H:12]([N:15]2[CH:19]=[C:18]([CH:20]=[O:21])[N:17]=[CH:16]2)[CH2:13][CH2:14]1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 2724141Tetrabutylammonium FluorideHCID 178455352HCID 178455352, 화합물

생성물 1

HCID 178519825HCID 178519825, 화합물수율 73.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

The compound (540 mg) obtained in Step 2 of this Reference Example was dissolved in tetrahydrofuran (8 mL). To this solution, a solution of tetrabutylammonium fluoride in tetrahydrofuran (1.0 M, 2.62 mL) was added, and the mixture was stirred at room temperature for 8 hours. To the reaction solution, saturated aqueous ammonium chloride was added, and organic matter was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. This crude product was purified by diol-bonded silica gel column chromatography (eluting solvent: hexane/ethyl acetate=1/1-ethyl acetate) to obtain the title compound (250 mg).

후처리

  1. extractionorganic matter was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. distillationthe solvent was distilled off under reduced pressure
  5. customto obtain a crude product
  6. customThis crude product was purified by diol-
  7. washsilica gel column chromatography (eluting solvent: hexane/ethyl acetate=1/1-ethyl acetate)

출처 및 근거

ORD 기록
ord-d51b1b7f3a2440d39b101467ef12b60e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609710B2

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