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4-Methoxybutanoyl chloride → HCID 77506366, 화합물

HRID 1712462
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HRID 1712462 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[NH:4][CH2:3][CH:2]1[CH2:11][O:12][CH:13]1[CH:18]([C:19]2[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH2:28][O:29][CH2:30][C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=3[O:37][CH3:38])=[CH:21][CH:20]=2)[CH2:17][CH2:16][N:15]([C:39]([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40])[CH2:14]1.[CH3:46][O:47][CH2:48][CH2:49][CH2:50][C:51](Cl)=[O:52]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[CH3:38][O:37][C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][C:31]=1[CH2:30][O:29][CH2:28][CH2:27][CH2:26][O:25][C:22]1[CH:23]=[CH:24][C:19]([CH:18]2[CH2:17][CH2:16][N:15]([C:39]([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40])[CH2:14][CH:13]2[O:12][CH2:11][CH:2]2[CH2:3][N:4]([C:51](=[O:52])[CH2:50][CH2:49][CH2:48][O:47][CH3:46])[C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=3[O:1]2)=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 127949894-Methoxybutanoyl chlorideHCID 77506189HCID 77506189, 화합물

생성물 1

HCID 77506366HCID 77506366, 화합물

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 8471Triethylamine용매

실험 절차

A solution of 0.33 g of tert-butyl 3-(3,4-dihydro-2H-benzo[1,4]oxazin-2(R,S)-ylmethoxy)-4-{4-[3-(2-methoxybenzyloxy)propoxy]phenyl}piperidine-1-carboxylate in 40 ml of chloroform and 0.23 ml of triethylamine is admixed at room temperature with 0.23 g of 4-methoxybutyryl chloride and stirred over 30 minutes. The reaction mixture is washed successively with 1N HCl and 1N NaOH, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a colourless oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.27 (1:1.5 EtOAc-heptane); Rt=6.05.

후처리

  1. washThe reaction mixture is washed successively with 1N HCl and 1N NaOH
  2. dry with materialdried over sodium sulphate
  3. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-531e0cfc4fbe449ca27bad2d8d2880b5
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790715B2

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