Water → HCID 13577656、化合物

HRID 1589206ノート

反応式

HRID 1589206 の反応式
[NH2:1][C:2]1[C:7]([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][C:18]([OH:20])=[O:19].[Na].O.[CH2:23](I)[CH3:24]>CN(C)C=O>[NH2:1][C:2]1[C:7]([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][C:18]([O:20][CH2:23][CH3:24])=[O:19]

参加物

6

反応物 4

HCID 962Water2 回HCID 6340IodoethaneHCID 5360545SodiumHCID 12901227HCID 12901227、化合物

生成物 1

HCID 13577656HCID 13577656、化合物収率 4.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3.12 g (0.1 mole) of 2-amino-3-benzoyl-5-chlorobenzeneacetic acid, sodium salt.1/2 H2O in 250 ml of dry dimethylformamide was treated with 44 g of ethyl iodide (0.3 mole) under nitrogen and stirred for 2 hours. The resulting solution was then added to one liter of water and extracted several times with ethyl ether. The combined ether layers were washed with water, dried over sodium sulfate, filtered and stripped to yield a solid yellow residue. This residue was recrystallized from ethyl alcohol, yielding 1.5 g of the title compound as yellow needles, m.p. 80°-82° C.

後処理

  1. extractionextracted several times with ethyl ether
  2. washThe combined ether layers were washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customto yield a solid yellow residue
  6. customThis residue was recrystallized from ethyl alcohol

出典と根拠

ORDレコード
ord-7e09a371909e438a9ee04b2cbbf3319d
出典データセット
uspto-grants-1986_02
特許番号
US04568695

反応ノート

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