2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 1,2,3,4-Tetrahydro-5,8-dimethoxy-2,3-dimethylene-1,4-epoxyanthracene

HRID 444402노트

반응식

HRID 444402 반응식
[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]2[C:4]=1[CH2:5][C:6]1[CH:7]3[O:19][CH:10]([C:11]=1[CH2:12]2)[C:9](=[CH2:20])[C:8]3=[CH2:21].ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[C:13]2[C:4]=1[CH:5]=[C:6]1[C:11](=[CH:12]2)[CH:10]2[O:19][CH:7]1[C:8](=[CH2:21])[C:9]2=[CH2:20]

참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 133409781,2,3,4,9,10-Hexahydro-5,8-dimethoxy-2,3-dimethylene-1,4-epoxyanthracene

생성물 1

HCID 126711181,2,3,4-Tetrahydro-5,8-dimethoxy-2,3-dimethylene-1,4-epoxyanthracene수율 98%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of 2 g (7.1 mmol) of 1,2,3,4,9,10-hexahydro-5,8-dimethoxy-2,3-dimethylene-1,4-epoxyanthracene, 1.77 g (7.8 mmol) of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone and 30 ml of benzene was stirred at room temperature under nitrogen for 30 minutes. The precipitate formed was filtered off and washed with benzene, the benzene solution was washed with two 30 ml portions of saturated aqueous sodium hydrogen sulphite solution and two 30 ml portions of water, dried over sodium sulphate and concentrated to dryness. By recrystallization from diethyl ether/tetrahydrofuran/methylene chloride (4:1:2) there were obtained 1.95 g (98%) of 1,2,3,4-tetrahydro-5,8-dimethoxy-2,3-dimethylene-1,4-epoxyanthracene of melting point 205°-206° C. in the form of white crystals.

후처리

  1. customThe precipitate formed
  2. filtrationwas filtered off
  3. washwashed with benzene
  4. washthe benzene solution was washed with two 30 ml portions of saturated aqueous sodium hydrogen sulphite solution and two 30 ml portions of water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated to dryness
  7. customBy recrystallization from diethyl ether/tetrahydrofuran/methylene chloride (4:1:2) there

출처 및 근거

ORD 기록
ord-ac066600761544b5bfb102d7d3b58451
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04264510

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