Sulfuric Acid → HCID 21427683、化合物

HRID 437996

反応式

HRID 437996 の反応式
S(=O)(=O)(O)O.[CH2:6]([C:8]1(O)[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH3:15])[CH3:7].[CH3:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][SH:23]>O>[CH2:6]([C:8]1([S:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH3:17])[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH3:15])[CH3:7]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 81061-HexanethiolHCID 2474821,2-Diethylcyclohexanol

生成物 1

HCID 21427683HCID 21427683、化合物収率 76%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
0 °C

実験手順

To a cooled (0° C.) mixture of water (13 ml.) and 27 mg. concentrated sulphuric acid was added dropwise 1,2-diethylcyclohexanol (12 g., 77 mmole) and then n-hexylthiol (9.1 g., 77 mmole). The mixture was stirred at 0° C. for 6 hours and at room temperature for 1 hour. The mixture was then poured into 1 liter of cold water and extracted with ether. The ether extract was washed with 2N sodium hydroxide and water and dried (MgSO4). The solvent was removed by distillation and the residue was distilled under reduced pressure to give n-hexyl 1,2-diethylcyclohexyl sulphide (15 g.) as a colourless liquid, b.p. 110°-4°/0.03 mm.

後処理

  1. temperatureTo a cooled
  2. extractionextracted with ether
  3. extractionThe ether extract
  4. washwas washed with 2N sodium hydroxide and water
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed by distillation
  7. distillationthe residue was distilled under reduced pressure

出典と根拠

ORDレコード
ord-67e7afc088a64bae962efaad97f1f6cf
出典データセット
uspto-grants-1977_06
特許番号
US04032661

関連ノート

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