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Hydrogen Bromide → 5-Bromo-2,2-difluoropentanoic acid

HRID 1249532
ノート
印刷プレビュー

反応式

HRID 1249532 の反応式
Br.[Br:2][CH2:3][CH2:4][CH2:5][C:6]([F:12])([F:11])[C:7]([O:9]C)=[O:8].CCOCC>O>[Br:2][CH2:3][CH2:4][CH2:5][C:6]([F:12])([F:11])[C:7]([OH:9])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 260Hydrogen Bromide3 回HCID 3283Diethyl EtherHCID 13769950Methyl 5-bromo-2,2-difluoropentanoate

生成物 1

HCID 137699515-Bromo-2,2-difluoropentanoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

HBr gas was introduced into 48% HBr in H2O (100 ml) with occasional cooling in an ice bath until the weight became 180 g. The HBr solution was then added to Part (5) compound (8.4 g, 36.3 mmole) at room temperature and the reaction was stirred for 5 hours at room temperature. The reaction was cooled to 0° C. and poured into Et2O (900 ml) in an ice bath. The products were extracted into the Et2O layer. The water layer was further extracted with Et2O (200 ml and 100 ml). The combined ether layers were washed with H2O (200 ml). The H2O wash was backwashed with Et2O (100 ml). The Et2O layers were combined and dried over MgSO4. Filtration and evaporation of solvent gave the title compound (7.8 g, quant.) as a colorless liquid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturewith occasional cooling in an ice bath until the weight
  2. temperatureThe reaction was cooled to 0° C.
  3. extractionThe products were extracted into the Et2O layer
  4. extractionThe water layer was further extracted with Et2O (200 ml and 100 ml)
  5. washThe combined ether layers were washed with H2O (200 ml)
  6. washThe H2O wash
  7. dry with materialdried over MgSO4
  8. filtrationFiltration and evaporation of solvent

出典と根拠

ORDレコード
ord-a430d0cba0e14f8ca42afa1c0278414b
出典データセット
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04632931

反応ノート

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