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Hydroxyamine hydrochloride → HCID 88359135, 화합물

HRID 2209732
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인쇄 미리보기

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HRID 2209732 반응식
[C:1]([C:3]1[CH:37]=[CH:36][C:6]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:14]2[CH:15]=[CH:16][C:17]([C:27]([N:29]([CH:33]([CH3:35])[CH3:34])[CH:30]([CH3:32])[CH3:31])=[O:28])=[C:18]([CH:26]=2)[O:19][C:20]([CH3:25])([CH3:24])[C:21]([OH:23])=[O:22])=[CH:5][CH:4]=1)#[N:2].Cl.[NH2:39][OH:40].[O-]CC.[Na+:44]>C(O)C>[Na+:44].[NH2:2][C:1](=[N:39][OH:40])[C:3]1[CH:4]=[CH:5][C:6]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][C:14]2[CH:15]=[CH:16][C:17]([C:27]([N:29]([CH:30]([CH3:32])[CH3:31])[CH:33]([CH3:35])[CH3:34])=[O:28])=[C:18]([CH:26]=2)[O:19][C:20]([CH3:25])([CH3:24])[C:21]([O-:23])=[O:22])=[CH:36][CH:37]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 2723922Sodium ethoxideHCID 19040993HCID 19040993, 화합물

생성물 1

HCID 88359135HCID 88359135, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

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온도
50 °C

실험 절차

A stirred solution of 2-[5-[5-(4-cyanophenoxy)pentyloxy]-2-[N,N-bis(1-methylethyl)aminocarbonyl]phenoxy]-2-methylpropionic acid (1.4 g, 2.8 mmol) in 30 mL of anhydrous ethanol is treated with hydroxylamine hydrochloride (590 mg, 8.4 mmol) and 21% sodium ethoxide solution in ethanol (3.1 mL, 5.7 mmol) and stirred at 50° C. overnight. The reaction is concentrated in vacuo and purified by chromatography on silica gel (20 g) with 80-100% ethyl acetate/hexane followed by 0-10% methanol/ethyl acetate as the eluent to afford 2-[5-[5-[4-[amino(hydroxyimino)methyl]phenoxy]pentyloxy]2-[N,N-bis(1-methylethyl) -aminocarbonyl]phenoxy]-2-methylpropanoic acid sodium salt as a colorless foam;

후처리

  1. concentrationThe reaction is concentrated in vacuo
  2. custompurified by chromatography on silica gel (20 g) with 80-100% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-b8d7a6124bee4678bcf6d64747c04c1e
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05455274

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