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Ammonium Acetate → 6-(Octadecylthio)hexanamide

HRID 634605
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HRID 634605 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium AcetateHCID 53857071HCID 53857071, 화합물

생성물 1

HCID 212601376-(Octadecylthio)hexanamide수율 79.9%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0e7a2c4815fd4a6fb2902c866077cf43
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06184180B2

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