Monoperoxyphthalic Acid Magnesium Salt → HCID 86613450, 화합물

HRID 507827노트

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HRID 507827 반응식
[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:32]=[CH:31][CH:30]=[CH:29][C:8]=1[C:9]([NH:11][CH2:12][C@H:13]([CH:26]([CH3:28])[CH3:27])[CH2:14][C@H:15]([NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])[CH:16]=[CH2:17])=[O:10].C(O[O-])(=O)C1C(=CC=CC=1)C([O-])=[O:37].[Mg+2]>CO>[CH3:1][O:2][CH2:3][CH2:4][CH2:5][O:6][C:7]1[CH:32]=[CH:31][CH:30]=[CH:29][C:8]=1[C:9]([NH:11][CH2:12][C@H:13]([CH:26]([CH3:27])[CH3:28])[CH2:14][C@H:15]([NH:18][C:19](=[O:25])[O:20][C:21]([CH3:23])([CH3:24])[CH3:22])[C@@H:16]1[CH2:17][O:37]1)=[O:10]

참가 물질

4

반응물 2

HCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 86613451tert-Butyl (3(S)-{[2-(3-methoxypropoxy)benzoylamino]methyl}-4-methyl-1(S)-vinylpentyl)carbamate

생성물 1

HCID 86613450HCID 86613450, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The solution of 1.48 g of tert-butyl (3(S)-{[2-(3-methoxypropoxy)benzoylamino]methyl}-4-methyl-1(S)-vinylpentyl)carbamate in 30 ml of methanol is admixed with 7.81 g of magnesium monoperoxyphthalate and stirred over 72 hours. The reaction mixture is poured onto water and extracted with tert-butyl methyl ether (2×). The combined organic phases are washed with water and brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained from the residue by means of flash chromatography (SiO2 60F) as a yellowish oil. Rf=0.30 (1:1 EtOAc-heptane, run 2×); Rt=18.64 (gradient II).

후처리

  1. additionThe reaction mixture is poured onto water
  2. extractionextracted with tert-butyl methyl ether (2×)
  3. washThe combined organic phases are washed with water and brine
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-1ed91074025e403d8d8a96b4629661c0
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786307B2

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