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

HRID 1669349
ノート
印刷プレビュー

反応式

HRID 1669349 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 694002-Methoxyethyl chloroformate2 回HCID 802933-Aminobenzyl alcohol

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b9f2c5aff96f4401aaf7bd87e2a21e9c
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989478B2

反応ノート

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