Sodium Hydroxide → HCID 117873508、化合物

HRID 64495ノート

反応式

HRID 64495 の反応式
[C:1]([O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]Cl)([CH3:4])([CH3:3])[CH3:2].NC(N)=[S:15].[OH-].[Na+]>O>[C:1]([O:5][CH:6]([SH:15])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 132806981-tert-Butoxy-6-chlorohexane

生成物 1

HCID 117873508HCID 117873508、化合物収率 76.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

After 73.2 g of 1-tert-butoxy-6-chlorohexane (0.38 mol), 38 g of thiourea (0.5 mol), and 30 ml of distilled water were put into a 500 ml two-necked flask equipped with a condenser and refluxed at 120° C. for 5 hours, a temperature was cooled to room temperature, and 300 ml of a previously prepared aqueous solution of NaOH (30 g) was added thereto and refluxed at 110° C. for 14 hours. The reactant was cooled to room temperature, the formed organic layer was extracted with ether and dried over MgSO4, and then the solvent was removed under reduced pressure, thereby obtaining 55.6 g of an oily product (6-tert-butoxyhexane-1-thiol, yield 76.9 mol %). Purity of the product confirmed through gas chromatography (GC) analysis was 97%, and results of proton nuclear magnetic resonance (1H-NMR) spectroscopy were as follows.

後処理

  1. customequipped with a condenser
  2. temperaturea temperature was cooled to room temperature
  3. temperaturerefluxed at 110° C. for 14 hours
  4. temperatureThe reactant was cooled to room temperature
  5. extractionthe formed organic layer was extracted with ether
  6. dry with materialdried over MgSO4
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-d3e03ff8f8ed413a8cc89a801345663d
出典データセット
uspto-grants-2016_09
特許番号
US09447211B2

反応ノート

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