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Ammonium Acetate → 6-(Octadecylthio)hexanamide

HRID 634605
ノート
印刷プレビュー

反応式

HRID 634605 の反応式
C([O-])(=O)C.[NH4+:5].[CH2:6]([S:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30](Cl)=[O:31])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]>CC(N(C)C)=O>[CH2:6]([S:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30]([NH2:5])=[O:31])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 53857071HCID 53857071、化合物

生成物 1

HCID 212601376-(Octadecylthio)hexanamide収率 79.9%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

In a 300 ml flask equipped with a stirrer, a condenser and a calcium chloride dryer tube were charged 19.3 g of ammonium acetate and 100 ml of DMAc, and the mixture was stirred at room temperature. Then, to the solution was gradually added dropwise 21.0 g of 6-(octadecylthio)hexanoic acid chloride and stirring of the mixture was continued for further 20 hours. The mixture was stirred at 60° C. for further 2 hours on a hot water bath. After cooling the reaction mixture to room temperature, the precipitated crystals were collected by filtration under reduced pressure and washed with acetone. The resulting crystals were collected by filtration under reduced pressure and washed with distilled water and recrystallized from IPA to obtain 16.0 g of the title compound as white crystals. Melting point: 105° C.

後処理

  1. customIn a 300 ml flask equipped with a stirrer, a condenser and a calcium chloride dryer tube
  2. stirringstirring of the mixture
  3. stirringThe mixture was stirred at 60° C. for further 2 hours on a hot water bath
  4. temperatureAfter cooling the reaction mixture to room temperature
  5. filtrationthe precipitated crystals were collected by filtration under reduced pressure
  6. washwashed with acetone
  7. filtrationThe resulting crystals were collected by filtration under reduced pressure
  8. washwashed with distilled water
  9. customrecrystallized from IPA

出典と根拠

ORDレコード
ord-0e7a2c4815fd4a6fb2902c866077cf43
出典データセット
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06184180B2

反応ノート

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