Water → Methyl acetyl(p-bromobenzoyl)acetate

HRID 553661

反応式

HRID 553661 の反応式
[CH3:1][O:2][C:3](=[O:9])[CH:4]=[C:5](NC)[CH3:6].N1C=CC=CC=1.[Br:16][C:17]1[CH:25]=[CH:24][C:20]([C:21](Cl)=[O:22])=[CH:19][CH:18]=1.[OH2:26]>C1COCC1>[CH3:1][O:2][C:3](=[O:9])[CH:4]([C:21](=[O:22])[C:20]1[CH:24]=[CH:25][C:17]([Br:16])=[CH:18][CH:19]=1)[C:5](=[O:26])[CH3:6]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 685154-Bromobenzoyl chlorideHCID 2734182Methyl 3-(methylamino)but-2-enoate

生成物 1

HCID 603116Methyl acetyl(p-bromobenzoyl)acetate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To 3-methylamino-but-2-enoic acid methyl ester (5.0 g, 39.1 mmol) in THF (70 mL) was added pyridine (3.7 mL, 47 mmol) dropwise. The mixture was cooled to 0° C., and 4-bromobenzoyl chloride (8.55 g, 39.1 mmol) in THF (30 mL) was added dropwise. The reaction was stirred at room temperature overnight, and then water was added. The mixture was extracted with EtOAc, and the combined organic layers were washed with water, dried, filtered, and concentrated to give the title compound.

後処理

  1. extractionThe mixture was extracted with EtOAc
  2. washthe combined organic layers were washed with water
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6b5161bf103c4a3fb0b47f7e1ce1a3b0
出典データセット
uspto-grants-2011_11
特許番号
US08048902B2

関連ノート

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