Hydrochloric Acid → Hexane, 2,5-dichloro-2,5-dimethyl-

HRID 1017159

反応式

HRID 1017159 の反応式
[ClH:1].[CH3:2][C:3](O)([CH2:5][CH2:6][C:7]([CH3:10])(O)[CH3:8])[CH3:4].C(Cl)[Cl:13]>>[Cl:1][C:3]([CH3:4])([CH2:5][CH2:6][C:7]([Cl:13])([CH3:10])[CH3:8])[CH3:2]

参加物

4

反応物 3

HCID 313Hydrochloric Acid3 回HCID 6344DichloromethaneHCID 80312,5-Dimethyl-2,5-hexanediol

生成物 1

HCID 80360Hexane, 2,5-dichloro-2,5-dimethyl-

反応条件

温度
0 °C

実験手順

A 2 L three neck round bottom flask fit with an overhead stirrer, thermometer, and nitrogen inlet was charged with 1.2 L concentrated HCl. The HCl was stirred land chilled in an ice/salt bath to 0° C. Gradually, 150 g of 2,5-dimethyl-2,5-hexanediol (Aldrich) was added to the HCl. The reaction mixture was initially a milky white slurry which gradually thickened and the ice bath was removed to allow the reaction to warm to 10 C. The solids were isolated by filtration, dissolved in methylene chloride (500 mL) and washed repeatedly with water until neutral to pH paper. The organics were dried over anhydrous magnesium sulfate and left in the refrigerator overnight. The resulting mixture stripped on the rotary evaporator to yield)of white crystalline 2,5-dichloro-2,5-dimethylhexane (152 g, 94% pure by GC). 1HNMR (CDCl3, 500 MHz) δ1.95 (s, 4H); 1.60 (s, 12H).

後処理

  1. customthe ice bath was removed
  2. customthe reaction
  3. temperatureto warm to 10 C
  4. customThe solids were isolated by filtration
  5. washwashed repeatedly with water until neutral
  6. dry with materialThe organics were dried over anhydrous magnesium sulfate
  7. customThe resulting mixture stripped on the rotary evaporator

出典と根拠

ORDレコード
ord-f7e021648d7f4ee1b8f9eb782d661ae2
出典データセット
uspto-grants-2002_11
特許番号
US06479424B1

関連ノート

読み込み中…