Sulfuric Acid → 3-(2',4'-Difluoro-4-biphenylyl)butane-1,3-diol

HRID 26928

反応式

HRID 26928 の反応式
[OH:1][CH2:2][CH2:3][C:4](=[O:6])[CH3:5].Br[C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=2[F:21])=[CH:10][CH:9]=1.[Mg].S(=O)(=O)(O)O>CCOCC>[F:21][C:15]1[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:14]=1[C:11]1[CH:12]=[CH:13][C:8]([C:4]([OH:6])([CH3:5])[CH2:3][CH2:2][OH:1])=[CH:9][CH:10]=1

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 1115094-Hydroxy-2-ButanoneHCID 5462224MagnesiumHCID 213226111,1'-Biphenyl, 4'-bromo-2,4-difluoro-

生成物 1

HCID 213225623-(2',4'-Difluoro-4-biphenylyl)butane-1,3-diol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

0.44 g. of 1 -hydroxy-3-butanone in 40 ml. of ether is added dropwise, at 20° to stirred Grignard solution obtained from 2.69 g. of 4-bromo-2',4'-difluorobiphenyl and 0.24 g. of magnesium in 100 ml. of ether. The mixture is stirred for two hours more and the resulting alcoholate is decomposed with dilute sulfuric acid. The ether phase is worked up in the customary manner to give 3-(2',4'-difluoro-4-biphenylyl)butane-1,3-diol, m.p. 82°-84°.

後処理

  1. customobtained from 2.69 g
  2. stirringThe mixture is stirred for two hours more

出典と根拠

ORDレコード
ord-d3e09d4998144f26af463aa41940b803
出典データセット
uspto-grants-1979_04
特許番号
US04151302

関連ノート

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