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Water → HCID 21476435, 화합물

HRID 2293155
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HRID 2293155 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10]([CH2:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[C:21]([NH:24][C:25]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=1[CH3:32])[N:20]=[C:19]2[N:33]1[CH2:42][CH2:41][C:40]2[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=2)[CH:34]1[CH3:43])=O)C.O>O1CCCC1>[OH:9][CH2:10][CH2:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[C:21]([NH:24][C:25]1[CH:30]=[CH:29][C:28]([F:31])=[CH:27][C:26]=1[CH3:32])[N:20]=[C:19]2[N:33]1[CH2:42][CH2:41][C:40]2[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=2)[CH:34]1[CH3:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 21476512HCID 21476512, 화합물

생성물 1

HCID 21476435HCID 21476435, 화합물수율 58.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of 0.12 g of lithium aluminium hydride (3.0 mM) and 30 ml of tetrahydrofuran, 1.5 g of the compound (3.0 mM) prepared in Step 2 dissolved in tetrahyrofuran was dropwise added at 0° C. and stirred for an hour. The reaction solution was added with water and extracted from dichloromethane. The dichloromethane layer was dehydrated, concentrated and purified by silica gel column chromatography, to give 0.80 g of the title compound.

후처리

  1. additionwas dropwise added at 0° C.
  2. extractionextracted from dichloromethane
  3. concentrationconcentrated
  4. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-29b68f0cd240489ab916b91450fc2b73
출처 데이터셋
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05686458

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