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Calcium Carbonate → 3-(N-2-hydroxyethyl-N-methylamino)benzonitrile

HRID 591140
ノート
印刷プレビュー

反応式

HRID 591140 の反応式
[CH3:1][NH:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[C:6]#[N:7].Br[CH2:12][CH2:13][OH:14].C([O-])([O-])=O.[Ca+2]>O>[OH:14][CH2:13][CH2:12][N:2]([CH3:1])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[C:6]#[N:7]
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 10112Calcium CarbonateHCID 108982-BromoethanolHCID 177940363-(Methylamino)benzonitrile

生成物 1

HCID 586560573-(N-2-hydroxyethyl-N-methylamino)benzonitrile収率 76.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3-methylaminobenzonitrile (11.36 g, 86 mmol, 1.0 eq), 2-bromoethanol (43.00 g, 344 mmol, 4.0 eq) and CaCO3 (34.40 g, 344 mmol, 4.0 eq) are added into water (150 ml) at room temperature, and the resulting mixture is refluxed with elevated temperature for 13.5 h, then cooled and filtered, and the aqueous solution is extracted with ethyl acetate (100 ml*3). The organic phases are combined, washed with water (20 ml*2), washed with saturated brine twice, dried over anhydrous sodium sulfate, and concentrated to give a light yellow oily crude product (11.55 g, crude yield: 76.2%). The crude product can be used directly in next step without purification.

後処理

  1. temperaturethe resulting mixture is refluxed with elevated temperature for 13.5 h
  2. temperaturecooled
  3. filtrationfiltered
  4. extractionthe aqueous solution is extracted with ethyl acetate (100 ml*3)
  5. washwashed with water (20 ml*2)
  6. washwashed with saturated brine twice
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-31b0e4c7b5044d5c854abf29dd9e66ae
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09238632B2

反応ノート

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