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Water → HCID 57425539, 화합물

HRID 2114366
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HRID 2114366 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]1([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH:12]=[CH:11][C:10]([C:13]([NH:22][C:23](=O)OC(C)(C)C)([CH3:21])[C:14](=O)[N:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:9][CH:8]=1.O.[F-].[Na+]>C1COCC1.C1(C)C=CC=CC=1>[C:7]1([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)[CH:12]=[CH:11][C:10]([C:13]([NH:22][CH3:23])([CH3:21])[CH2:14][N:15]2[CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:9][CH:8]=1
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참가 물질

7

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HCID 962WaterHCID 5235Sodium FluorideHCID 21226445Aluminium lithium hydrideHCID 57488852HCID 57488852, 화합물

생성물 1

HCID 57425539HCID 57425539, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 8028
Tetrahydrofuran
용매

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온도
0 °C

실험 절차

LAH (447 mg, 11.8 mmol ) was added to a solution of 1,1-dimethylethyl [1-(4-biphenylyl)-1-methyl-2-oxo-2-(1-pyrrolidinyl)ethyl]carbamate (580 mg, 1.47 mmol) in THF (20 ml) at 0° C. under argon. The resulting mixture was then refluxed for 2.5 h. The reaction mixture was then cooled in and ice bath and diluted with toluene (20 ml). Water (847 ul, 47 mmol) was added followed by NaF (1.48 g, 35.3 mmol) and the mixture was stirred at 0° C. for 30 min, filtered and the filter pad was washed with THF. The combined filtrates were concentrated to give 417 mg (96%) as a light brown oil. MS(ES) m/e 295.4 [M+H]+

후처리

  1. temperatureThe resulting mixture was then refluxed for 2.5 h
  2. temperatureThe reaction mixture was then cooled in and ice bath
  3. filtrationfiltered
  4. washthe filter pad was washed with THF
  5. concentrationThe combined filtrates were concentrated
  6. customto give 417 mg (96%) as a light brown oil

출처 및 근거

ORD 기록
ord-7631cf695c1f4f17afac865d55df710d
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432258B2

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