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Hydrochloric Acid → HCID 67593801, 화합물

HRID 865308
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HRID 865308 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:13])[CH2:8][S:9][CH2:10]2)=[CH:5][CH:4]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[F:24][C:25]([F:34])([F:33])[C:26](C1NC=CN=1)=[O:27].Cl>O1CCCC1>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=[O:13])[CH:8]([C:26](=[O:27])[C:25]([F:34])([F:33])[F:24])[S:9][CH2:10]2)=[CH:5][CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 313Hydrochloric AcidHCID 3232557-Methoxy-1H-isothiochromen-4(3H)-oneHCID 5654362,2,2-Trifluoro-1-(1H-imidazol-2-yl)ethanoneHCID 2724254Sodium bis(trimethylsilyl)amide

생성물 1

HCID 67593801HCID 67593801, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

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온도
-78 °C

실험 절차

7-Methoxyisothiochroman-4-one from Step 3 (0.58 g, 3.0 mmol) was dissolved in tetrahydrofuran (30 mL) and cooled to -78° C. A solution of sodium bistrimethylsilylamide (3.0 mL of a 1.0M tetrahydrofuran solution) was added and the reaction stirred for 0.5 hours at -78° C. Trifluoroacetyl imidazole (0.41 mL, 3.6 mmol) was added and the reaction was warmed to room temperature and stirred under a nitrogen atmosphere for 16 hours. At this time, 1N hydrochloric acid (200 mL) was added to the reaction followed by extraction with ether (250 mL). The organics were washed with brine (150 mL), dried over MgSO4 and concentrated in vacuo. The resulting yellow oil (0.42 g, 48%) was used without further purification.

후처리

  1. temperaturethe reaction was warmed to room temperature
  2. stirringstirred under a nitrogen atmosphere for 16 hours
  3. extractionfollowed by extraction with ether (250 mL)
  4. washThe organics were washed with brine (150 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customThe resulting yellow oil (0.42 g, 48%) was used without further purification

출처 및 근거

ORD 기록
ord-535d7ced92f240aeaa55ce919b9e359f
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05565482

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