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Tetrahydrofuran → HCID 12800412、化合物

HRID 543556
ノート
印刷プレビュー

反応式

HRID 543556 の反応式
[CH:1](NC1CCCCC1)([CH3:3])[CH3:2].C([Li])CCC.[CH2:16]([CH:19]1[N:22]([C:23]([C:43]([O:45][CH2:46][C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)=[O:44])=[P:24]([C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=2)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:21](=[O:53])[CH2:20]1)[CH:17]=[CH2:18].[O:54]1CCCC1>CCCCCC>[CH2:16]([CH:19]1[N:22]([C:23]([C:43]([O:45][CH2:46][C:47]2[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=2)=[O:44])=[P:24]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[C:21](=[O:53])[CH:20]1[C:1]([OH:54])([CH3:3])[CH3:2])[CH:17]=[CH2:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 62386CyclohexylisopropylamineHCID 127969694-Allyl-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl)azetidin-2-oneHCID 178418339Butyllithium

生成物 1

HCID 12800412HCID 12800412、化合物

試薬・触媒・溶媒 1

HCID 8058
Hexane
溶媒

実験手順

A solution of N-isopropylcyclohexylamine (0.60 g) in dry tetrahydrofuran (10 cm3) was stirred under argon and cooled to -78°. This was treated with a 2.5 M solution of n-butyl lithium in n-hexane (1.70 cm3). After ten minutes, a solution of 4-allyl-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl) azetidin-2-one (1.00 g) in dry tetrahydrofuran (15 cm3) was added. Five minutes were allowed for the formation of the C(3) carbanion which was then quenched by the addition of dry acetone (0.71 cm3). The cooling bath was then removed and the mixture stirred for a further ten minutes before it was neutralised with acetic acid (0.56 g). The solvent was evaporated under reduced pressure and the residue chromatographed on silica gel 60 (<230 mesh), eluting with ethyl acetate/60°-80° petroleum ether mixtures grading from 1:1 to 7:3. this gave the two separate isomers of 4-allyl-3-(2-hydroxyprop-2-yl)-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl)azetidin-2-one(0.30 g 27%) and (0.22 g, 20%); νmax (CHCl3) 3000, 1735 and 1620 cm-1.

後処理

  1. temperaturecooled to -78°
  2. waitAfter ten minutes
  3. customFive minutes
  4. customwas then quenched by the addition of dry acetone (0.71 cm3)
  5. customThe cooling bath was then removed
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue chromatographed on silica gel 60 (<230 mesh)
  8. washeluting with ethyl acetate/60°-80° petroleum ether
  9. customthis gave the two
  10. customseparate isomers of 4-allyl-3-(2-hydroxyprop-2-yl)-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl)azetidin-2-one(0.30 g 27%) and (0.22 g, 20%)

出典と根拠

ORDレコード
ord-87e9a1eb450045e28b13eda5c7f213d8
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04446146

反応ノート

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