1,6-Dibromohexane → HCID 105201、化合物

HRID 1828214ノート

反応式

HRID 1828214 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7]Br.[S:9]([O-:12])([O-:11])=[O:10].[Na+].[Na+]>O>[CH2:2]([S:9]([OH:12])(=[O:11])=[O:10])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][S:9]([OH:12])(=[O:11])=[O:10]

参加物

4

反応物 2

HCID 123681,6-DibromohexaneHCID 24437Sodium Sulfite

生成物 1

HCID 105201HCID 105201、化合物収率 100%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1,6-dibromohexane (25 ml, 0.16 mol) and sodium sulfite (45.5 g, 0.36 mol) in water (85 ml) were heated at reflux for 16 h. The mixture was then filtered whilst hot and the filtrate was concentrated under reduced pressure to yield the hexane 1,6-disulfonic acid (39.3 g, 0.16 mol) which was used without further purification. The diacid was ground into a fine powder and powdered phosphorus pentachloride (84 g, 0.4 mol) was added carefully. After an initial vigorous reaction, the mixture was heated with mechanical stirring at 110° C. for 90 min., yielding a mustard coloured solution. On cooling the mixture was cautiously triturated with ice/water and the resultant solid filtered off. The solid was washed with water and dried under vacuum to afford the disulfonyl chloride hexane compound as a cream yellow solid (38.6 g, 96%). This material was used without purification in the next step.

後処理

  1. temperatureat reflux for 16 h
  2. filtrationThe mixture was then filtered whilst hot and the filtrate
  3. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-7eb182d74a984dcd8bb177b47eb7c4cf
出典データセット
uspto-grants-2006_06
特許番号
US07056987B2

反応ノート

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