Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluoro-10-iodo- → 1,1,2,2-Tetrahydroperfluorodecanethiol

HRID 1936976

반응식

HRID 1936976 반응식
N[C:2](N)=[S:3].[F:5][C:6]([F:32])([CH2:29]CI)[C:7]([F:28])([F:27])[C:8]([F:26])([F:25])[C:9]([F:24])([F:23])[C:10]([F:22])([F:21])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14]>C(O)C>[F:5][C:6]([F:32])([CH2:29][CH2:2][SH:3])[C:7]([F:27])([F:28])[C:8]([F:25])([F:26])[C:9]([F:23])([F:24])[C:10]([F:21])([F:22])[C:11]([F:20])([F:19])[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14]

참가 물질

4

반응물 2

HCID 74885Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluoro-10-iodo-HCID 2723790Thiourea

생성물 1

HCID 5427551,1,2,2-Tetrahydroperfluorodecanethiol수율 93.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of thiourea (105.7 g, 1.39 moles), 2-(perfluorooctyl)ethyl iodide (531.5 g), 0.926 moles) and anhydrous ethanol (1000 mL) was heated at reflux for 6 hours. Approximately half of the alcohol was removed at reduced pressure and replaced with water. Solid sodium hydroxide (37.0 g) was added and the mixture heated under slow nitrogen purge. The volatile liquid products were collected by steam distillation using a modified Dean-Stark apparatus to yield 414 g (93.1 molar yield) of 2-(perfluorooctyl)ethyl mercaptan. After two consecutive water washes the product was suficiently pure by glc (99.3%) and used without further purification.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 6 hours
  3. customApproximately half of the alcohol was removed at reduced pressure
  4. additionSolid sodium hydroxide (37.0 g) was added
  5. temperaturethe mixture heated under slow nitrogen
  6. custompurge
  7. distillationThe volatile liquid products were collected by steam distillation

출처 및 근거

ORD 기록
ord-8992845735af4df482151e6c00fc53ea
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06391948B1

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