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Cyclohexylisopropylamine → HCID 20461593, 화합물

HRID 1703042
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HRID 1703042 반응식
[CH:1](NC1CCCCC1)(C)C.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]>O1CCCC1.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[CH3:1])[CH:17]=[CH2:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 20461593HCID 20461593, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회
HCID 8058
Hexane
용매

실험 절차

A solution of N-isopropylcyclohexylamine (0.30 g) in dry tetrahydrofuran (5 ml) was stirred under argon and cooled to -78°. This was treated with a 2.5 M solution of n-butyl lithium in hexane (0.85 ml) and stirred for 10 minutes. A solution of 4-allyl-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl)azetidine-2-one (9) (0.50 g) in tetrahydrofuran (5 ml) was added and after 5 minutes the anion was quenched by addition of methyl iodide (0.12 ml). After a period of 10 minutes the reaction vessel was transferred to an ice bath and a further 10 minutes later the reaction was neutralized by addition of acetic acid (0.16 ml). The solvent was then stripped off and the residue partitioned between ethyl acetate and brine. The ethyl acetate solution was separated, washed with brine and dried over sodium sulphate. The product was subjected to careful column chromatography on silica gel 60 eluting with cyclohexane/ethyl acetate mixtures grading from 1:1 to 3:7. This gave 4-allyl-3-methyl-1-(1-benzyloxycarbonyl-1-triphenylphosphoranylidenemethyl)azetidine-2-one (38) (0.10 g, 19%); νmax (CHCl3) 3000, 1735 and 1610 cm-1. Running closely behind this was recovered starting phosphorane (9) (0.17 g. 33%).

후처리

  1. temperaturecooled to -78°
  2. customwas quenched by addition of methyl iodide (0.12 ml)
  3. waitAfter a period of 10 minutes the reaction vessel was transferred to an ice bath and a further 10 minutes
  4. additionlater the reaction was neutralized by addition of acetic acid (0.16 ml)
  5. customthe residue partitioned between ethyl acetate and brine
  6. customThe ethyl acetate solution was separated
  7. washwashed with brine
  8. dry with materialdried over sodium sulphate
  9. customthis was recovered

출처 및 근거

ORD 기록
ord-f137394a74ae4af39f0dc56277d6e41c
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04350703

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