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

反応式

HRID 1936976 の反応式
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]

参加物

4

反応物 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

生成物 1

HCID 5427551,1,2,2-Tetrahydroperfluorodecanethiol収率 93.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8992845735af4df482151e6c00fc53ea
出典データセット
uspto-grants-2002_05
特許番号
US06391948B1

関連ノート

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