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Oxalyl chloride → Ethyl 6-[o-[p-(4-phenylbutoxy)benzamido]phenyl]hexanate

HRID 982222
ノート
印刷プレビュー

反応式

HRID 982222 の反応式
[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:20]=[CH:19][C:15]([C:16](Cl)=[O:17])=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C1(CCCCOC2C=CC(C(O)=O)=CC=2)C=CC=CC=1.C(Cl)(=O)C(Cl)=O.[NH2:47][C:48]1[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=1[CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][C:59]([O:61][CH2:62][CH3:63])=[O:60]>C(Cl)Cl.N1C=CC=CC=1>[C:1]1([CH2:7][CH2:8][CH2:9][CH2:10][O:11][C:12]2[CH:20]=[CH:19][C:15]([C:16]([NH:47][C:48]3[CH:53]=[CH:52][CH:51]=[CH:50][C:49]=3[CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][C:59]([O:61][CH2:62][CH3:63])=[O:60])=[O:17])=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 65578Oxalyl chlorideHCID 110438254-(4-Phenylbutoxy)benzoic AcidHCID 11055348Benzoyl chloride, 4-(4-phenylbutoxy)-HCID 19882678Ethyl 6-(o-aminophenyl)hexanate

生成物 1

HCID 19882682Ethyl 6-[o-[p-(4-phenylbutoxy)benzamido]phenyl]hexanate

試薬・触媒・溶媒 2

HCID 1049
Pyridine
溶媒
HCID 6344Dichloromethane溶媒

実験手順

A solution of p-(4-phenylbutoxy)benzoyl chloride prepared from 1 g of p-(phenylbutoxy)benzoic acid and 2 ml of oxalyl chloride in methylene chloride was added to a solution of 0.6 g of ethyl 6-(o-aminophenyl)hexanate obtained in Reference Example 17 in 10 ml of pyridine at temperature less than -30° C. The mixture was stirred at room temperature overnight and concentrated under reduced pressure. Toluene was added to the residue. The mixture was washed with diluted hydrochloric acid and then with water and dried over anhydrous magnesium sulfate. The systems was concentrated under reduced pressure to obtain 1.0 g of oily ethyl 6-[o-[p-(4-phenylbutoxy)benzamido]phenyl]hexanate.

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionToluene was added to the residue
  3. washThe mixture was washed with diluted hydrochloric acid
  4. dry with materialwith water and dried over anhydrous magnesium sulfate
  5. concentrationThe systems was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-d0b8c9280db245309a2280d90b6aa51b
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04994479

反応ノート

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