m-Chloroperbenzoic acid → HCID 91035818, 화합물

HRID 561882노트

반응식

HRID 561882 반응식
[Cl:1][C:2]1[C:3]([CH2:13][N:14]([CH:47]2[CH2:49][CH2:48]2)[C:15](=[O:46])[CH:16]([CH2:26][C:27]2[CH:32]=[CH:31][C:30]([O:33][CH2:34][CH2:35][O:36][C:37]3[C:42]([Cl:43])=[CH:41][C:40]([CH3:44])=[CH:39][C:38]=3[Cl:45])=[CH:29][CH:28]=2)[CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][O:11][CH3:12])=[N:6][CH:7]=1.ClC1C=C(C=CC=1)C(OO)=[O:55]>ClCCl>[Cl:1][C:2]1[C:3]([CH2:13][N:14]([CH:47]2[CH2:48][CH2:49]2)[C:15](=[O:46])[CH:16]([CH2:26][C:27]2[CH:28]=[CH:29][C:30]([O:33][CH2:34][CH2:35][O:36][C:37]3[C:42]([Cl:43])=[CH:41][C:40]([CH3:44])=[CH:39][C:38]=3[Cl:45])=[CH:31][CH:32]=2)[CH2:17][NH:18][C:19](=[O:25])[O:20][C:21]([CH3:22])([CH3:23])[CH3:24])=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][O:11][CH3:12])=[N+:6]([O-:55])[CH:7]=1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 91185349Tert-butyl (3-[{[5-chloro-2-(methoxypropyl)pyridin-4-yl]methyl}(cyclopropyl)amino]-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}-3-oxopropyl)carbamate

생성물 1

HCID 91035818HCID 91035818, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl (3-[{[5-chloro-2-(methoxypropyl)pyridin-4-yl]methyl}(cyclopropyl)amino]-2-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]benzyl}-3-oxopropyl)carbamate from Experiment 94, Step 4 in dichloromethane (0.03 M) was added 3-chloroperoxybenzoic acid. The reaction mixture was stirred at RT for 16 h. The reaction was quenched with water and then extracted with EtOAc. The combined organic extracts were washed with 10% aq. HCl and brine, dried over MgSO4, filtered and the filtrate concentrated in vacuo. Purification of the crude product thus obtained by way of flash chromatography (SiO2, 1:1 (v/v) Hex:EtOAc 4 EtOAc) afforded the title compound.

후처리

  1. customThe reaction was quenched with water
  2. extractionextracted with EtOAc
  3. washThe combined organic extracts were washed with 10% aq. HCl and brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationthe filtrate concentrated in vacuo
  7. customPurification of the crude product
  8. customthus obtained by way of flash chromatography (SiO2, 1:1 (v/v) Hex:EtOAc 4 EtOAc)

출처 및 근거

ORD 기록
ord-7bbd7ad74d934fc1ab4d2d4d5643c0ac
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063105B2

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