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1,8-Diazabicyclo(5.4.0)undec-7-ene → Tert butyl 4-iodo-1-methyl-7-oxo-6-azabicyclo[3.2.1]oct-3-ene-6-carboxylate

HRID 74996
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인쇄 미리보기

반응식

HRID 74996 반응식
[I:1][CH:2]1[CH:8]2[CH2:9][C:5]([CH3:18])([C:6](=[O:17])[N:7]2[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:4][CH2:3]1.N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1>[I:1][C:2]1[CH:8]2[CH2:9][C:5]([CH3:18])([C:6](=[O:17])[N:7]2[C:10]([O:12][C:13]([CH3:15])([CH3:14])[CH3:16])=[O:11])[CH2:4][CH:3]=1
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참가 물질

4

반응물 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 68008486Tert-butyl 4-iodo-1-methyl-7-oxo-6-azabicyclo[3.2.1]octane-6-carboxylate2회

생성물 1

HCID 86667435Tert butyl 4-iodo-1-methyl-7-oxo-6-azabicyclo[3.2.1]oct-3-ene-6-carboxylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of tert-butyl 4-iodo-1-methyl-7-oxo-6-azabicyclo[3.2.1]octane-6-carboxylate, 52d, (7.6 g, 20.8 mmol) in 100 mL of toluene was added 1,8-diazabicyclo[5.4.0]undec-7-ene (6.2 mL, 41.6 mmol). The reaction was warmed to reflux and stirred overnight. The reaction was concentrated in vacuo and the resulting residue was purified by silica gel chromatography (4:1 Hexanes:EtOAc), yielding 4.9 g of the desired product, 52e.

후처리

  1. temperatureThe reaction was warmed
  2. temperatureto reflux
  3. concentrationThe reaction was concentrated in vacuo
  4. customthe resulting residue was purified by silica gel chromatography (4:1 Hexanes:EtOAc)

출처 및 근거

ORD 기록
ord-f6ec80e78160492bb71c71bd04ea671f
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829007B2

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