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Suprofen → HCID 3642305、化合物

HRID 461742
ノート
印刷プレビュー

反応式

HRID 461742 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5359SuprofenHCID 6328Methyl iodideHCID 12679HexamethylphosphoramideHCID 5360545Sodium

生成物 1

HCID 3642305HCID 3642305、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e625c0631464f868e7cefe89069014c
出典データセット
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04064132

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート