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Cyclohexylisopropylamine → HCID 20461593、化合物

HRID 1388287
ノート
印刷プレビュー

反応式

HRID 1388287 の反応式
[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]
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 3

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

生成物 1

HCID 20461593HCID 20461593、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 8058
Hexane
溶媒

実験手順

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.-1Running closely behind this was recovered starting phosphorane (9) (0.17 g. 33%).

後処理

  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. custom-1Running closely behind this was recovered

出典と根拠

ORDレコード
ord-726f12acb8404876b528977577a8eb3b
出典データセット
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04431587

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート