Sulfuric Acid → HCID 14180572、化合物

HRID 1904960ノート

反応式

HRID 1904960 の反応式
[CH2:1]1[CH2:10][O:9][C:8]2[C:7](=[O:11])[CH:6]=[CH:5][C:4](=[O:12])[C:3]=2[O:2]1.[CH2:13]=[CH:14][C:15]([Cl:17])=[CH2:16].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].S(=O)(=O)(O)O>C(O)(=O)C.O>[Cl:17][C:15]1[CH:16]=[C:5]2[C:6](=[CH:13][CH:14]=1)[C:7](=[O:11])[C:8]1[O:9][CH2:10][CH2:1][O:2][C:3]=1[C:4]2=[O:12]

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 25408Sodium DichromateHCID 31369ChloropreneHCID 140804552,3-Dihydro-1,4-benzodioxine-5,8-dione

生成物 1

HCID 14180572HCID 14180572、化合物収率 71.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒2 回

実験手順

A mixture of 2,3-ethylenedioxy-1,4-benzoquinone (17 g) and freshly distilled chloroprene (13 g) in glacial acetic acid (100 mL) was stirred at ambient temperature for 90 hours. The mixture was then diluted with additional acetic acid (500 mL) followed by the addition of a solution of sodium dichromate (40 g) and sulfuric acid (2 mL) in water (25 mL). The mixture was heated at 60° -70°C. for 2 hours, then cooled and diluted with water (500 mL). The resulting bright orange precipitate was collected and dried to yield 18.25 g of 6-chloro-2,3-ethylenedioxy-1,4-naphthoquinone, mp 279°-80° C.

後処理

  1. temperatureThe mixture was heated at 60° -70°C. for 2 hours
  2. temperaturecooled
  3. customThe resulting bright orange precipitate was collected
  4. customdried

出典と根拠

ORDレコード
ord-26d9489be7e54a978c1255c7e64210fd
出典データセット
uspto-grants-1989_06
特許番号
US04840965

反応ノート

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