Water → 63805-96-9

HRID 436760

反応式

HRID 436760 の反応式
[S-:1][C:2]#[N:3].[Na+].[C:5]([N:9]=[N:10][C:11](Cl)([CH2:13][CH:14]([CH3:16])[CH3:15])[CH3:12])([CH3:8])([CH3:7])[CH3:6].O>C(O)(C)C>[C:5]([N:9]=[N:10][C:11]([N:3]=[C:2]=[S:1])([CH2:13][CH:14]([CH3:16])[CH3:15])[CH3:12])([CH3:8])([CH3:7])[CH3:6]

参加物

5

反応物 3

HCID 962WaterHCID 516871Sodium thiocyanateHCID 23344796(E)-1-tert-Butyl-2-(2-chloro-4-methylpentan-2-yl)diazene

生成物 1

HCID 2143116863805-96-9

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
30 °C

実験手順

To a stirred solution of 26.1 grams (0.3 moles) of sodium thiocyanate in 150 ml of 75% aqueous isopropanol in a 500 ml erlenmeyer flask, cooled to 5° C., was added 61.2 grams (0.3 moles) of 2-t-butylazo- 2-chloro-4-methylpentane holding the reaction temperature at 10°-20° C. After the addition was complete, the reaction mixture was stirred an additional two hours at 30° C., poured into 300 ml water and the product extracted with 200 ml pentane. The pentane extract was washed with water, 10% NaHCO3 solution, dried over anhydrous sodium sulfate, filtered and the pentane evaporated under reduced pressure to leave 55.7 grams (80% crude yield) of a yellow liquid. The product had a strong broad band at 1980- 2080 cm-1 in its infrared spectrum which is indicative of the isothiocyano band.

後処理

  1. additionAfter the addition
  2. extractionthe product extracted with 200 ml pentane
  3. extractionThe pentane extract
  4. washwas washed with water, 10% NaHCO3 solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe pentane evaporated under reduced pressure
  8. customto leave 55.7 grams (80% crude yield) of a yellow liquid

出典と根拠

ORDレコード
ord-d5c486a9375c4a3fb176a4ef4a256d07
出典データセット
uspto-grants-1977_06
特許番号
US04028344

関連ノート

読み込み中…