1,6-Dibromohexane → HCID 105201, 화합물

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.

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

ORD 기록

ord-7eb182d74a984dcd8bb177b47eb7c4cf

출처 데이터셋

uspto-grants-2006_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07056987B2