Sodium perfluorobutanesulfonate → HCID 178448399、化合物

HRID 1168023ノート

反応式

HRID 1168023 の反応式
C(OP([O-])(OCC)=O)C.[C:10]([IH+:14]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:13])([CH3:12])[CH3:11].[F:25][C:26]([F:41])([S:37]([O-:40])(=[O:39])=[O:38])[C:27]([F:36])([F:35])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30].[Na+]>O>[F:41][C:26]([F:25])([S:37]([O-:40])(=[O:39])=[O:38])[C:27]([F:35])([F:36])[C:28]([F:34])([F:33])[C:29]([F:32])([F:31])[F:30].[C:21]([IH+:14]([C:10]([CH3:13])([CH3:12])[CH3:11])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:24])([CH3:23])[CH3:22]

参加物

4

反応物 2

HCID 23678450Sodium perfluorobutanesulfonateHCID 178448396HCID 178448396、化合物

生成物 1

HCID 178448399HCID 178448399、化合物収率 90.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Di-tert-butylphenyliodonium diethylphosphate (546 mg; 1 mmol) and sodium perfluorobutanesulfonate (354 mg; 1.1 mmol) were dissolved in water (10 ml), and the resultant mixture was extracted three times with methylene chloride (10 ml). The solvent was removed through distillation, and precipitated white solid was washed with ether, followed by recrystallization from a mixture of methylene chloride and ether, to thereby precipitate 561 mg of the target compound as white crystals (yield: 81%).

後処理

  1. extractionthe resultant mixture was extracted three times with methylene chloride (10 ml)
  2. customThe solvent was removed through distillation
  3. customprecipitated white solid
  4. washwas washed with ether
  5. customfollowed by recrystallization from a mixture of methylene chloride and ether

出典と根拠

ORDレコード
ord-6f78140de4bd437eadeadc7a1aa1a9ea
出典データセット
uspto-grants-2003_09
特許番号
US06620957B1

反応ノート

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