Acetic Acid → HCID 23150364、化合物

HRID 550330ノート

反応式

HRID 550330 の反応式
[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

参加物

6

反応物 3

HCID 176Acetic AcidHCID 2658432,7-dibromophenanthrene-9,10-dioneHCID 178418332HCID 178418332、化合物

生成物 1

HCID 23150364HCID 23150364、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c4a7e11ef2d44a2c8591bb5c18ab2929
出典データセット
uspto-grants-2011_05
特許番号
US07947382B2

反応ノート

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