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Ethyl Acetate → 3-[(2-Methoxyethoxy)carbonylamino]benzyl alcohol

HRID 1669349
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HRID 1669349 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].Cl[C:11]([O:13][CH2:14][CH2:15][O:16][CH3:17])=[O:12].C(OCC)(=O)C>O1CCCC1>[CH3:17][O:16][CH2:15][CH2:14][O:13][C:11]([NH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6])=[O:12]
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참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 694002-Methoxyethyl chloroformate2회HCID 802933-Aminobenzyl alcohol

생성물 1

HCID 673477703-[(2-Methoxyethoxy)carbonylamino]benzyl alcohol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 15.0 g of 3-aminobenzyl alcohol in 120 ml of tetrahydrofuran was added dropwise a solution of 18 ml of 2-methoxyethyl chloroformate in 70 ml of tetrahydrofuran under ice-cooling. After stirred for 30 minutes under ice-cooling and then at room temperature for 30 minutes, additional 2 ml of 2-methoxyethyl chloroformate was added, and the mixture was stirred at room temperature for 1 hour. After ethyl acetate was added, the mixture was washed successively with an aqueous saturated sodium bicarbonate solution and then an aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated to obtain 30.2 g of 3-[(2-methoxyethoxy)carbonylamino]benzyl alcohol.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. waitat room temperature for 30 minutes
  4. stirringthe mixture was stirred at room temperature for 1 hour
  5. washthe mixture was washed successively with an aqueous saturated sodium bicarbonate solution
  6. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b9f2c5aff96f4401aaf7bd87e2a21e9c
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07989478B2

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