1,2-Dichloroethane → HCID 4415129、化合物

HRID 383983ノート

反応式

HRID 383983 の反応式
C1C=NC2N(O)N=NC=2C=1.[F:11][C:12]1[CH:20]=[CH:19][C:15]([CH2:16][CH2:17][NH2:18])=[CH:14][CH:13]=1.[C:21](O)(=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(Cl)CCl>C(Cl)Cl>[F:11][C:12]1[CH:20]=[CH:19][C:15]([CH2:16][CH2:17][NH:18][C:21](=[O:28])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[CH:14][CH:13]=1

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 243Benzoic AcidHCID 4653p-FluorophenethylamineHCID 181649HOAt

生成物 1

HCID 4415129HCID 4415129、化合物収率 78%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

1.5 g (10.8 mmol) of HOAt were added to a solution of 15.0 g (108.0 mmol) of 4-fluorophenethylamine and 13.2 g (108.0 mmol) of benzoic acid in DCM and the mixture was then cooled to 0° C. 22.8 g (119.0 mmol) of EDC were then added at this temperature and the mixture was then stirred for 16 h at RT. The reaction solution was then washed successively with a 1M aqueous hydrochloric acid (2×300 ml), a 2M aqueous NaOH solution (300 ml) and brine (200 ml). The organic phase was dried over Na2SO4, filtered and concentrated to small volume under vacuum. 20.5 g (84.2 mmol, 78%) of N-(4-fluorophenethyl)benzamide were obtained as the residue.

後処理

  1. washThe reaction solution was then washed successively with a 1M aqueous hydrochloric acid (2×300 ml)
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated to small volume under vacuum

出典と根拠

ORDレコード
ord-e8b30a8aca7a4a76b1dfa733f16b4ddc
出典データセット
uspto-grants-2013_02
特許番号
US08367700B2

反応ノート

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