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Nitric Acid → HCID 14802112, 화합물

HRID 329714
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HRID 329714 반응식
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:4]([C:15]([O:17][CH3:18])=[O:16])[CH:3]=1.[N+:19]([O-])([OH:21])=[O:20]>S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:14]=[C:13]([N+:19]([O-:21])=[O:20])[C:5]([O:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:4]([C:15]([O:17][CH3:18])=[O:16])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 2728538Methyl 5-chloro-2-(2-ethoxy-2-oxoethoxy)benzoate

생성물 1

HCID 14802112HCID 14802112, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

실험 절차

A solution of 620 g of ethyl 4-chloro-2-methoxycarbonylphenoxyacetate in 1600 ml of concentrated sulfuric acid is cooled below 0° C, and a mixture of 102 ml of fuming nitric acid (d 1.50) and 102 ml of concentrated sulfuric acid is added dropwise below 5° C. The resultant solution is stirred for 3 hours under ice-cooling and poured into ice-cold water and then extracted with ethyl acetate. The extract is washed with water twice and dried over magnesium sulfate. The solvent is distilled off and the residue is gradually crystallized to give 697 g of ethyl 4-chloro-2-methoxycarbonyl-6-nitrophenoxyacetate, melting at 68°-70° C.

후처리

  1. additionis added dropwise below 5° C
  2. temperaturecooling
  3. additionpoured into ice-cold water
  4. extractionextracted with ethyl acetate
  5. washThe extract is washed with water twice
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent is distilled off
  8. customthe residue is gradually crystallized

출처 및 근거

ORD 기록
ord-1e2bbc488004447785c3731202cc5b44
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04892872

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