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Diethyl Ether → HCID 14698589, 화합물

HRID 846214
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HRID 846214 반응식
[CH3:1][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20](OCC)=[O:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].C(OCC)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O>[CH3:4][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][OH:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:1])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 14698592HCID 14698592, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 14698589HCID 14698589, 화합물수율 25%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.2 g. (6.2 mMol) of the compound prepared in Example 31 in 50 ml. dry diethyl ether are heated with 1 g. lithium aluminium hydride, subsequently poured into water and a little 10% sulphuric acid, extracted with diethyl ether, dried over anhydrous sodium sulphate, filtered and the solvent removed in a vacuum. The residue is then recrystallised from toluene to give the title compound in a yield of 25% of theory; m.p. 136°-142° C.

후처리

  1. extractiona little 10% sulphuric acid, extracted with diethyl ether
  2. dry with materialdried over anhydrous sodium sulphate
  3. filtrationfiltered
  4. customthe solvent removed in a vacuum
  5. customThe residue is then recrystallised from toluene

출처 및 근거

ORD 기록
ord-bf293de67bf54b31a40e8ad1aeafe602
출처 데이터셋
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05135949

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