Bromide ion → 2-(Trifluoromethyl)benzhydryl bromide

HRID 1720852ノート

反応式

HRID 1720852 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:16]=[CH:15][CH:14]=[CH:13][C:4]=1[CH:5](O)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.P(Br)(Br)[Br:20].[Br-]>C(OCC)C>[F:1][C:2]([F:18])([F:17])[C:3]1[CH:16]=[CH:15][CH:14]=[CH:13][C:4]=1[CH:5]([Br:20])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 259Bromide ionHCID 24614Phosphorus tribromideHCID 27774012-(Trifluoromethyl)benzhydrol

生成物 1

HCID 224164932-(Trifluoromethyl)benzhydryl bromide

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

2-(Trifluoromethyl)benzhydrol (20.2 g, 79.9 mmol) was dissolved in ethyl ether (195 mL), and cooled in an ice-H2O bath, under N2. To the resulting solution was added, dropwise, a solution of PBr3 (3.80 mL, 40.0 mmol) in ethyl ether (95 mL). After addition was complete, the reaction mixture was brought to room temperature and stirred for 16 hours. The reaction mixture was cooled in an ice-H2O bath and quenched with H2O (200 mL). The aqueous layer was extracted with ethyl ether (2×200 mL). The combined organic extracts were dried (MgSO4), filtered, and concentrated to dryness at low heat to give a quantitative yield of product bromide as a pale yellow oil. 300 MHz 1H NMR (CDCl3): δ6.69 (s, 1H, (Ph)2CH. MS: 235 (M+ -Br).

後処理

  1. temperaturecooled in an ice-H2O bath, under N2
  2. additionTo the resulting solution was added
  3. additionAfter addition
  4. customwas brought to room temperature
  5. temperatureThe reaction mixture was cooled in an ice-H2O bath
  6. customquenched with H2O (200 mL)
  7. extractionThe aqueous layer was extracted with ethyl ether (2×200 mL)
  8. dry with materialThe combined organic extracts were dried (MgSO4)
  9. filtrationfiltered
  10. concentrationconcentrated to dryness
  11. temperatureat low heat

出典と根拠

ORDレコード
ord-d6bbe4e9d4cb47f2a44983397c5c7d8f
出典データセット
uspto-grants-1996_04
特許番号
US05508273

反応ノート

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