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Water → HCID 53930828, 화합물

HRID 248419
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HRID 248419 반응식
[CH3:1][O:2][CH2:3][C:4]([NH2:6])=[S:5].[CH2:7]([O:9][C:10](=[O:16])[CH:11](Cl)[C:12]([CH3:14])=O)[CH3:8].O>C1C=CC=CC=1.C(OCC)(=O)C>[CH2:7]([O:9][C:10]([C:11]1[S:5][C:4]([CH2:3][O:2][CH3:1])=[N:6][C:12]=1[CH3:14])=[O:16])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 962WaterHCID 11858Ethyl 2-chloroacetoacetateHCID 203233692-Methoxyethanethioamide

생성물 1

HCID 53930828HCID 53930828, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 8857Ethyl Acetate용매

실험 절차

20 g of methoxythioacetamide are added, with vigorous stirring, to 31.3 g of 2-chloroacetoacetic acid ethyl ester in 400 ml of benzene at room temperature and then, using a water separator, heated under reflux for 41/2 hours. After cooling to room temperature, the benzenic reaction solution is diluted with 500 ml of ethyl acetate, washed twice using 80 ml of 10% sodium carbonate solution each time and twice using 50 ml of water each time, dried over sodium sulfate and filtered. The solvent mixture is evaporated off. The yellow oil that remains is crystallised by trituration with diisopropyl ether. The beige-coloured crystals melt at 36°-37° C.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 41/2 hours
  3. washwashed twice
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customThe solvent mixture is evaporated off
  7. customThe yellow oil that remains is crystallised by trituration with diisopropyl ether
  8. custommelt at 36°-37° C.

출처 및 근거

ORD 기록
ord-0ea164d80e204d7686d68b1b233b3b2b
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05210205

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