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(Diethylamino)sulfur trifluoride → HCID 59389366, 화합물

HRID 2357926
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HRID 2357926 반응식
CCN(S(F)(F)[F:7])CC.O[C:11]([C:14]1[CH:32]=[C:17]2[C:18]([C:24]3[CH:25]([CH3:31])[CH2:26][C:27](=[O:30])[NH:28][N:29]=3)=[CH:19][CH:20]=[C:21]([O:22][CH3:23])[N:16]2[N:15]=1)([CH3:13])[CH3:12]>C(Cl)(Cl)Cl>[F:7][C:11]([C:14]1[CH:32]=[C:17]2[C:18]([C:24]3[CH:25]([CH3:31])[CH2:26][C:27](=[O:30])[NH:28][N:29]=3)=[CH:19][CH:20]=[C:21]([O:22][CH3:23])[N:16]2[N:15]=1)([CH3:13])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 123472(Diethylamino)sulfur trifluorideHCID 59389308HCID 59389308, 화합물

생성물 1

HCID 59389366HCID 59389366, 화합물수율 72.6%

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
0 °C

실험 절차

DAST (27.9 mg) was added dropwise to a solution of the compound of Example 242 (21.9 mg) in chloroform (5.0 mL) and the mixture was stirred at 0° C. for 30 min. Subsequently, the reaction was quenched by adding a saturated aqueous sodium bicarbonate solution and the mixture was extracted with chloroform (30 mL). The extract was washed with water and saturated brine and dried over anhydrous sodium sulfate. The dried extract was concentrated and purified by silica gel column chromatography (hexane:ethyl acetate=1:3→ :4) to afford the title compound as a colorless powder (16.0 mg).

후처리

  1. customSubsequently, the reaction was quenched
  2. additionby adding a saturated aqueous sodium bicarbonate solution
  3. extractionthe mixture was extracted with chloroform (30 mL)
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. extractionThe dried extract
  7. concentrationwas concentrated
  8. custompurified by silica gel column chromatography (hexane:ethyl acetate=1:3→ :4)

출처 및 근거

ORD 기록
ord-30a14e11a8dd4f869918d223e292f751
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07763617B2

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