Acetic Acid → HCID 86722263、化合物

HRID 869417ノート

反応式

HRID 869417 の反応式
[NH2:1][C:2]1[C:6]2[C:7]([Br:13])=[C:8]([O:11][CH3:12])[CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:14](=[O:28])[CH:15]=[CH:16][C:17]1[N:18]=[C:19]([NH:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[S:20][CH:21]=1.CC#N.CC(O)=O.OP(O)(O)=O>[Cl-].[Cl-].[Zn+2].O>[Br:13][C:7]1[C:6]2[C:2]3[NH:1][CH:16]([C:17]4[N:18]=[C:19]([NH:22][C:23](=[O:27])[CH:24]([CH3:26])[CH3:25])[S:20][CH:21]=4)[CH2:15][C:14](=[O:28])[C:3]=3[O:4][C:5]=2[CH:10]=[CH:9][C:8]=1[O:11][CH3:12]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 1004Phosphoric AcidHCID 6342AcetonitrileHCID 86722262HCID 86722262、化合物

生成物 1

HCID 86722263HCID 86722263、化合物収率 55.1%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of 16A (2 g, 4.3 mmol), ZnCl2 (6 g), MeCN (10 mL), AcOH (2 mL) and H3PO4 (2 mL) was heated to 90° C. and reacted overnight. TLC monitored the reaction. After the reaction completed, the reaction mixture was added dropwise into water, extracted with ethyl acetate and concentrated to give 16B (1.1 g, 55% yield).

後処理

  1. customreacted overnight
  2. customthe reaction
  3. extractionextracted with ethyl acetate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-7357f5891e964d5ab3ca22ae9acd37d7
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

読み込み中…