Hydrochloric Acid → 2-Chloro-2-methyl-3-nitrosopentane

HRID 1779749

反応式

HRID 1779749 の反応式
[ClH:1].[N:2]([O:4]CCC(C)C)=O.[CH3:10][C:11](=[CH:13][CH2:14][CH3:15])[CH3:12]>>[Cl:1][C:11]([CH3:12])([CH3:10])[CH:13]([N:2]=[O:4])[CH2:14][CH3:15]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 122432-Methyl-2-pentene

生成物 1

HCID 122253792-Chloro-2-methyl-3-nitrosopentane

反応条件

温度
5 °C

実験手順

Concentrated HCl (9.0 mL, 0.11 mol) was added to a cooled (0°-5° C.) solution of isoamyl nitrite (14.8 g, 0.1 mol) and 2-methyl-2-pentene (8.4 g, 0.1 mol). The temperature was maintained below 5° C. during the addition and the reaction mixture was stirred at 5° C. for an additional 30 min. The product was filtered and washed with a cold (-20° C.) 1:1 mixture of petroleum ether. The solid was further washed with petroleum ether to afford a white solid. Yield: 4.9 g (34%); mp 85°-86° C. 1H NMR (CDCl3) ε 0.98 (CH2CH3), 1.68 (d, 6H, CH3), 2.05 (m, 2H, CH2CH3), 5.88 (dd, 1H, CHNO). MS: 299 (2M+H)+. Anal. Calcd. for C6H12NOCl: C, 48.17; H, 8.08; N, 9.36, Cl,23.70. Found: C, 48.47; H, 8.33; N, 9.3, Cl,24.04.

後処理

  1. temperatureThe temperature was maintained below 5° C. during the addition
  2. filtrationThe product was filtered
  3. washwashed with a cold (-20° C.) 1:1 mixture of petroleum ether
  4. washThe solid was further washed with petroleum ether
  5. customto afford a white solid

出典と根拠

ORDレコード
ord-982b99839ad240a7b662ea1f7b400239
出典データセット
uspto-grants-1997_05
特許番号
US05627286

関連ノート

読み込み中…