Triethylamine → HCID 178483602、化合物

HRID 2276007ノート

反応式

HRID 2276007 の反応式
[CH3:1][NH:2][C:3]([CH3:9])=[CH:4][C:5]([O:7][CH3:8])=[O:6].C(N(CC)CC)C.[Cl:17][C:18]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:19]=1[C:20](Cl)=[O:21]>C1(C)C=CC=CC=1>[Cl:17][C:18]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:19]=1[C:20](=[O:21])[C:4](=[C:3]([NH:2][CH3:1])[CH3:9])[C:5]([O:7][CH3:8])=[O:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2734182Methyl 3-(methylamino)but-2-enoate2 回HCID 27365462-Chloro-4-fluorobenzoyl chloride

生成物 1

HCID 178483602HCID 178483602、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
2.5 °C

実験手順

To a mixture of methyl 3-(methylamino)-2-butenoate (i.e. the product of Step A) (10.25 g, 79.43 mmol) and triethylamine (13.26 mL, 9.63 g, 95.31 mmol) in toluene (125 mL) at 0° C. was added dropwise 2-chloro-4-fluorobenzoyl chloride (15.25 g, 79.48 mol) in toluene (25 mL) over 30 minutes while maintaining the temperature of the reaction mixture between about 0 to 5° C. The reaction mixture was allowed to warm to room temperature and stirred over night. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The resulting dark yellow oil was triturated with hexanes and filtered to provide the title compound as a white solid (15.91 g).

後処理

  1. temperatureto warm to room temperature
  2. filtrationThe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe resulting dark yellow oil was triturated with hexanes
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-9547ead4b53c4edc8253179d4ae48f9b
出典データセット
uspto-grants-2015_09
特許番号
US09131693B2

反応ノート

読み込み中…