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Suprofen → HCID 3642305, 화합물

HRID 461742
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HRID 461742 반응식
[C:1]1([C:6]([C:8]2[CH:18]=[CH:17][C:11]([CH:12]([CH3:16])[C:13]([OH:15])=[O:14])=[CH:10][CH:9]=2)=[O:7])[S:5][CH:4]=[CH:3][CH:2]=1.[Na].[CH3:20]N(C)P(N(C)C)(N(C)C)=O.CI>O>[C:1]1([C:6]([C:8]2[CH:18]=[CH:17][C:11]([CH:12]([CH3:16])[C:13]([O:15][CH3:20])=[O:14])=[CH:10][CH:9]=2)=[O:7])[S:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5359SuprofenHCID 6328Methyl iodideHCID 12679HexamethylphosphoramideHCID 5360545Sodium

생성물 1

HCID 3642305HCID 3642305, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred mixture of 28.2 parts of p-(2-thenoyl)hydratropic acid, sodium salt and 250 parts of hexamethylphosphoramide are added 56.8 parts of methyl iodide at room temperature (slightly exothermic reaction). The whole is stirred at room temperature for 1 hour. The reaction mixture is poured onto 1000 parts of water and the product is extracted three times with 140 parts of diisopropylether. The combined extracts are washed with 200 parts of water, dried, filtered and evaporated. The residue is crystallized from 35 parts of diisopropylether at 0° C, washed with cooled ether and dried, yielding methyl p-(2-thenoyl)hydratropate; mp. 62° C.

후처리

  1. customslightly exothermic reaction)
  2. extractionthe product is extracted three times with 140 parts of diisopropylether
  3. washThe combined extracts are washed with 200 parts of water
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue is crystallized from 35 parts of diisopropylether at 0° C
  8. washwashed with cooled ether
  9. customdried

출처 및 근거

ORD 기록
ord-3e625c0631464f868e7cefe89069014c
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04064132

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