Propargyl alcohol → HCID 19967853、化合物

HRID 975748ノート

反応式

HRID 975748 の反応式
[F:1][C:2]1[C:7]([C:8]2[C:13]([F:14])=[C:12]([F:15])[C:11]([F:16])=[C:10]([F:17])[C:9]=2[F:18])=[C:6]([F:19])[C:5]([F:20])=[C:4](F)[C:3]=1[F:22].[CH2:23]([OH:26])[C:24]#[CH:25].C(=O)([O-])[O-].[K+].[K+].C1OCCOCCOCCOCCOCCOC1>C1(C)C=CC=CC=1>[CH2:23]([O:26][C:4]1[C:5]([F:20])=[C:6]([F:19])[C:7]([C:8]2[C:13]([F:14])=[C:12]([F:15])[C:11]([F:16])=[C:10]([F:17])[C:9]=2[F:18])=[C:2]([F:1])[C:3]=1[F:22])[C:24]#[CH:25]

参加物

6

反応物 4

HCID 7859Propargyl alcoholHCID 11430Potassium CarbonateHCID 2855718-Crown-6HCID 67949Decafluorobiphenyl

生成物 1

HCID 19967853HCID 19967853、化合物収率 48%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of decafluorobiphenyl (1.67 g, 5 mmol), propargyl alcohol (0.58 ml), potassium carbonate (7.5 g), and 18-crown-6 (0.1 g) in 30 ml of toluene was stirred under reflux for 8 hours. After cooling to room temperature, 2 g of celite was added and the reaction mixture was filtered. The filtrate was evaporated on a rotavapor to remove most of the solvent and then the product was purified by preparative gas chromatography, giving 0.93 g (48%) of 4-Propargyloxynonafluorobiphenyl which was used in the next step.

後処理

  1. temperatureunder reflux for 8 hours
  2. addition2 g of celite was added
  3. filtrationthe reaction mixture was filtered
  4. customThe filtrate was evaporated on a rotavapor
  5. customto remove most of the solvent
  6. customthe product was purified by preparative gas chromatography

出典と根拠

ORDレコード
ord-2333b95d77de4177833553bccd738ca9
出典データセット
uspto-grants-1997_03
特許番号
US05610020

反応ノート

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