Dichloromethane → HCID 131733156、化合物

HRID 1525795ノート

反応式

HRID 1525795 の反応式
[CH2:1]([C:16]1[CH:22]=[CH:21][C:19]([NH2:20])=[CH:18][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].[C:23](=[O:26])([O-])[O-:24].[K+].[K+].Cl[CH2:30]Cl>ClC(OC)=O.O>[CH3:30][O:24][C:23](=[O:26])[NH:20][C:19]1[CH:18]=[CH:17][C:16]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15])=[CH:22][CH:21]=1

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 713745384-Pentadecylaniline

生成物 1

HCID 131733156HCID 131733156、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6586Methyl chloroformate溶媒

実験手順

To the solution of 4-pentadecanylaniline (3.4 g) in dichloromethane (60 mL), methyl chloroformate (1.1 mL) and the solution of potassium carbonate (7.8 g) in water (110 mL) were added at 0° C., followed by stirring at room temperature for 14 hours. The reaction solution was poured to water, followed by extraction with dichloroethane. The organic layer was washed sequentially with 2N hydrochloric acid, water and an aqueous saturated sodium chloride solution, and dried with anhydrous magnesium sulfate. The reaction solution was concentrated under reduced pressure to obtain the title compound (3.9 g) having the following physical property values.

後処理

  1. extractionfollowed by extraction with dichloroethane
  2. washThe organic layer was washed sequentially with 2N hydrochloric acid, water
  3. dry with materialan aqueous saturated sodium chloride solution, and dried with anhydrous magnesium sulfate
  4. concentrationThe reaction solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-13fd395f19c3494abcaa9807e6014fc5
出典データセット
uspto-grants-2015_07
特許番号
US09085523B2

反応ノート

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