Acetic Acid → HCID 23150364, 화합물

HRID 550330노트

반응식

HRID 550330 반응식
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[C:6](=[O:17])[C:5](=O)[C:4]=2[CH:3]=1.C[Mg]Cl.[C:22]([OH:25])(=O)[CH3:23]>C1COCC1.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:13]2[C:12]3[C:7](=[CH:8][C:9]([Br:16])=[CH:10][CH:11]=3)[C:6]([OH:17])([CH3:5])[C:22]([OH:25])([CH3:23])[C:14]=2[CH:15]=1

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 2658432,7-dibromophenanthrene-9,10-dioneHCID 178418332HCID 178418332, 화합물

생성물 1

HCID 23150364HCID 23150364, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

34.3 g (94 mmol) of 2,7-dibromophenanthrene-9,10-quinone were suspended in 600 ml of dry THF at −10° C. under argon, and 141 ml (282 mmol) of methylmagnesium chloride (2 molar solution in THF) were added dropwise at such a rate that the internal temperature did not exceed 0° C. The mixture was subsequently stirred overnight at room temperature. 50 ml of glacial acetic acid were added to the batch with ice cooling, and the mixture was diluted with ethyl acetate. After washing twice with saturated sodium chloride solution, the mixture was dried over sodium sulfate, and the solvents were removed, giving 43.4 g of the product, which was employed without further purification for the next step.

후처리

  1. customdid not exceed 0° C
  2. washAfter washing twice with saturated sodium chloride solution
  3. dry with materialthe mixture was dried over sodium sulfate
  4. customthe solvents were removed

출처 및 근거

ORD 기록
ord-c4a7e11ef2d44a2c8591bb5c18ab2929
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947382B2

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