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Hydrazine hydrate (1:1) → [2-(2-Methoxyethoxy)-ethyl]-hydrazine

HRID 12901
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HRID 12901 반응식
O.[NH2:2][NH2:3].Br[CH2:5][CH2:6][O:7][CH2:8][CH2:9][O:10][CH3:11]>C(O)C>[CH3:11][O:10][CH2:9][CH2:8][O:7][CH2:6][CH2:5][NH:2][NH2:3]
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 1235321-Bromo-3,6-dioxaheptane

생성물 1

HCID 18959038[2-(2-Methoxyethoxy)-ethyl]-hydrazine수율 85%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of hydrazine monohydrate (44.0 mL, 1.00 mol) in ethanol (75 mL) at 0° C. in an ice-water bath was added 1-(2-bromoethoxy)-2-methoxyethane (13.6 mL, 0.100 mol) drop-wise over 20 minutes. The reaction was then allowed to warm to room temperature and stir for 5 minutes and then heated to 40° C. in a preheated oil bath for 12 hours. The reaction was then cooled to room temperature and concentrated to remove the ethanol. The remaining aqueous layer was extracted with methylene chloride (2×100 mL) and diethyl ether (2×100 mL). The organic layers were combined and dried over anhydrous Na2SO4, filtered and concentrated to provide [2-(2-methoxyethoxy)-ethyl]-hydrazine as a light yellow oil (10.29 g, 85%).

후처리

  1. temperatureheated to 40° C. in a preheated oil bath for 12 hours
  2. temperatureThe reaction was then cooled to room temperature
  3. concentrationconcentrated
  4. customto remove the ethanol
  5. extractionThe remaining aqueous layer was extracted with methylene chloride (2×100 mL) and diethyl ether (2×100 mL)
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1759ce57e6de40e986407126f2e925cc
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07728029B2

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