Water → HCID 13577656, 화합물

HRID 1589206노트

반응식

HRID 1589206 반응식
[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]

참가 물질

6

반응물 4

HCID 962Water2회HCID 6340IodoethaneHCID 5360545SodiumHCID 12901227HCID 12901227, 화합물

생성물 1

HCID 13577656HCID 13577656, 화합물수율 4.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7e09a371909e438a9ee04b2cbbf3319d
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04568695

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