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Sodium Hydroxide → HCID 53720923, 화합물

HRID 2209736
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HRID 2209736 반응식
[C:1]([C:3]1[CH:31]=[CH:30][C:6]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:27]=[CH:26][C:16]([C:17]([N:19]([CH:23]([CH3:25])[CH3:24])[CH:20]([CH3:22])[CH3:21])=[O:18])=[CH:15][C:14]=2[O:28][CH3:29])=[CH:5][CH:4]=1)#[N:2].[OH-:32].[Na+].Cl.[NH2:35]O>O.C(O)C>[NH2:2][C:1](=[N:35][OH:32])[C:3]1[CH:4]=[CH:5][C:6]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:27]=[CH:26][C:16]([C:17]([N:19]([CH:23]([CH3:24])[CH3:25])[CH:20]([CH3:21])[CH3:22])=[O:18])=[CH:15][C:14]=2[O:28][CH3:29])=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 19381508HCID 19381508, 화합물

생성물 1

HCID 53720923HCID 53720923, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A stirred solution of 4-[4-(4-cyanophenoxy)butoxy]-3-methoxy-N,N-bis(1-methylethyl)benzamide (500 mg, 1.18 mmol) in 2 mL of water and 8 mL of ethanol is treated with sodium hydroxide (57.7 mg, 1.34 mmol) and hydroxylamine hydrochloride (90 mg, 1.29 mmol). After refluxing overnight, the reaction is partitioned between dichloromethane and brine. The organic phase is dried over magnesium sulfate, and concentrated in vacuo. The resulting material is purified by chromatography on silica gel (15 g) with ethyl acetate as the eluent to afford 4- [4-[4-[amino(hydroxyimino)methyl]phenoxy]butoxy]-3-methoxy-N,N-bis(1-methylethyl)benzamide as colorless crystals, mp=63°-65° C.;

후처리

  1. temperatureAfter refluxing overnight
  2. customthe reaction is partitioned between dichloromethane and brine
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe resulting material is purified by chromatography on silica gel (15 g) with ethyl acetate as the eluent

출처 및 근거

ORD 기록
ord-1e8ef46ba0c841189464530b77dab8a0
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05455274

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