Sulfuric Acid → HCID 14180572, 화합물

HRID 1904960노트

반응식

HRID 1904960 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 14180572HCID 14180572, 화합물수율 71.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 962Water용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-26d9489be7e54a978c1255c7e64210fd
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04840965

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