Azobisisobutyronitrile → 4-Acetylthio-1,1-bis(trifluoromethyl)-1-butanol

HRID 1353025

反応式

HRID 1353025 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]([C:8]([F:11])([F:10])[F:9])([OH:7])[CH2:4][CH:5]=[CH2:6].[C:14]([OH:17])(=[S:16])[CH3:15].CC(N=NC(C#N)(C)C)(C#N)C>N(C(C)(C)C#N)=NC(C)(C)C#N.O1CCOCC1>[C:14]([S:16][CH2:6][CH2:5][CH2:4][C:3]([C:8]([F:9])([F:10])[F:11])([C:2]([F:12])([F:13])[F:1])[OH:7])(=[O:17])[CH3:15]

参加物

6

反応物 3

HCID 6547Azobisisobutyronitrile2 回HCID 3288704-Penten-2-ol, 1,1,1-trifluoro-2-(trifluoromethyl)-HCID 178418634HCID 178418634、化合物2 回

生成物 1

HCID 865942984-Acetylthio-1,1-bis(trifluoromethyl)-1-butanol収率 80%

試薬・触媒・溶媒 2

HCID 6547Azobisisobutyronitrile触媒HCID 312751,4-Dioxane溶媒

実験手順

Under a nitrogen atmosphere, 20 g of 4,4-bis (trifluoromethyl)-4-hydroxy-1-butene (96.1 mmol), 8.05 g of thioacetic acid (105.7 mmol), 60 g of 1,4-dioxane and 0.79 g of 2,2′-azobisisobutyronitrile (hereinafter abbreviated as AIBN) (4.8 mmol) were put into a flask equipped with a stirring bar, a thermometer and a condenser, and heated with stirring. During the reaction, thioacetic acid and AIBN were appropriately added and after confirming that a substrate was completely consumed, the reaction solution was distilled as it was under reduced pressure to yield an intermediate product, 22 g of 4-acetylthio-1,1-bis (trifluoromethyl)-1-butanol (76.9 mmol).

後処理

  1. customwere put into a flask
  2. customequipped with a stirring bar
  3. temperaturea thermometer and a condenser, and heated
  4. additionwere appropriately added
  5. customwas completely consumed
  6. distillationthe reaction solution was distilled as it

出典と根拠

ORDレコード
ord-c3a9232ff3174da6924bb1a6f9bbcc87
出典データセット
uspto-grants-2007_05
特許番号
US07220808B2

関連ノート

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