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Ethyl chloroformate → HCID 21243401、化合物

HRID 621614
ノート
印刷プレビュー

反応式

HRID 621614 の反応式
[CH3:1][N:2]([CH2:4][CH:5]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:17])([F:16])[F:15])=[CH:10][CH:9]=1)C.Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27]>C1(C)C=CC=CC=1>[C:26]([N:2]([CH2:4][CH:5]([CH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]([F:15])([F:16])[F:17])=[CH:10][CH:9]=1)[CH3:1])([O:28][CH2:29][CH3:30])=[O:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 13653935N,N-dimethyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine

生成物 1

HCID 21243401HCID 21243401、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of N,N-dimethyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine (22.0 g) and ethyl chloroformate (34.1 g, 30.0 ml) in dry toluene (200 ml) is refluxed for 72 hours. The reaction mixture is cooled to room temperature, and the solvent removed under reduced pressure. Water (200 ml) is added, and the mixture extracted with dichloromethane (2×150 ml). The combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml), and dried over magnesium sulfate. The solvent is removed under reduced pressure to give N-carbethoxy-N-methyl-2-benzyl-3-(4-trifluoromethylphenoxy)propylamine as an oil, which is used without purification for the next synthetic step above.

後処理

  1. customthe solvent removed under reduced pressure
  2. additionWater (200 ml) is added
  3. extractionthe mixture extracted with dichloromethane (2×150 ml)
  4. washThe combined dichloromethane extracts are washed with 2N hydrochloric acid (200 ml) and water (200 ml)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is removed under reduced pressure

出典と根拠

ORDレコード
ord-ba8245c1ff80494b9eea00a9ef24cb99
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04824868

反応ノート

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