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HCID 19389968, 화합물 → HCID 19389970, 화합물

HRID 1757149
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HRID 1757149 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]1([C:20](O)=[O:21])[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[CH2:11][CH2:10][CH2:9]1>CCOC(C)=O>[NH2:7][C:8]1([CH2:20][OH:21])[C:17]2[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=2)[CH2:11][CH2:10][CH2:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 19389968HCID 19389968, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19389970HCID 19389970, 화합물수율 83.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of 172 mg (0.00452 mol) of lithium aluminum hydride in 6 mL of THY at 0° C. was added portion-wise 500 mg (0.00226 mol) of the product of Step B. The mixture was refluxed overnight. EtOAc was carefully added to quench excess hydride and 50% aqueous NaOH added. The mixture was extracted with EtOAc and the EtOAc extract washed with brine. It was dried (MgSO4) and concentrated to give an oil which solidified on standing to give 390 mg of a tan solid: mp 89°-95.6° C. 1H NMR (DMSO-d6) d 7.422 (d, 1H), 6.70 (d, 1H), 6.95 (s, 1H), 3.690 (s, 3H), 3.20-3.40 (m, 3H), 2.70 (t, 2H), 2.0-2.20 (m. 2H), 1.70 (m, 2H).

후처리

  1. temperatureThe mixture was refluxed overnight
  2. customto quench excess hydride and 50% aqueous NaOH
  3. additionadded
  4. extractionThe mixture was extracted with EtOAc
  5. extractionthe EtOAc extract
  6. washwashed with brine
  7. dry with materialIt was dried (MgSO4)
  8. concentrationconcentrated
  9. customto give an oil which

출처 및 근거

ORD 기록
ord-2ab3d13ad6144816af7b7f231439f7df
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05444079

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