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Triethylamine → HCID 21867225、化合物

HRID 857159
ノート
印刷プレビュー

反応式

HRID 857159 の反応式
[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([O:12][C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[CH:15][CH:14]=2)=[C:7]([Cl:27])[CH:6]=1.C(N(CC)CC)C.[C:36](Cl)(=[O:40])[CH:37]([CH3:39])[CH3:38]>ClCCl>[CH3:1][O:2][C:3](=[O:28])[CH2:4][C:5]1[CH:10]=[C:9]([Cl:11])[C:8]([O:12][C:13]2[CH:14]=[CH:15][C:16]([N:19]([C:36](=[O:40])[CH:37]([CH3:39])[CH3:38])[CH2:20][C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=3)=[CH:17][CH:18]=2)=[C:7]([Cl:27])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 62325Isobutyryl chlorideHCID 21867255Methyl[3,5-dichloro-4-(4-benzylaminophenoxy)phenyl]acetate

生成物 1

HCID 21867225HCID 21867225、化合物収率 95.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred mixture of methyl[3,5-dichloro-4-(4-benzylaminophenoxy)phenyl]acetate (0.36 g), triethylamine (0.10 g) and dichloromethane (40 mL) was added isobutyryl chloride (0.15 g). After 16 hours at room temperature, the reaction mixture was concentrated, and the residue partioned between ethyl acetate and water. The organic phase was washed with hydrochloric acid (1 N), a saturated aqueous solution of sodium hydrogencarbonate and brine. After concentration, the residue was purified on column (silica gel, petrolium ether/ethyl acetate, 4:1) to give, to give 0.40 g of methyl[3,5-dichloro-4-(4-(2-methylpropanoyl-benzylamino)phenoxy)phenyl]acetate.

後処理

  1. concentrationthe reaction mixture was concentrated
  2. washThe organic phase was washed with hydrochloric acid (1 N)
  3. concentrationAfter concentration
  4. customthe residue was purified on column (silica gel, petrolium ether/ethyl acetate, 4:1)
  5. customto give

出典と根拠

ORDレコード
ord-9ab1c2dfbffe470dbb877b766a4f2d38
出典データセット
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07144909B2

反応ノート

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