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Acetonitrile → HCID 20358774, 화합물

HRID 2082930
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HRID 2082930 반응식
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([NH2:12])=[CH:4][C:3]=1[C:13]([NH:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]([CH2:29][CH3:30])([CH3:28])[CH3:27])=[CH:22][C:21]=1[C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])=[O:14].[Cl:36][C:37]([Cl:42])([Cl:41])[C:38](Cl)=[O:39].C(N(CC)CC)C.C(#N)C>O>[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[C:5]([NH:12][C:38](=[O:39])[C:37]([Cl:42])([Cl:41])[Cl:36])=[CH:4][C:3]=1[C:13]([NH:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]([CH2:29][CH3:30])([CH3:27])[CH3:28])=[CH:22][C:21]=1[C:31]([CH2:34][CH3:35])([CH3:33])[CH3:32])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 6420Trichloroacetyl chlorideHCID 8471TriethylamineHCID 12525034HCID 12525034, 화합물

생성물 1

HCID 20358774HCID 20358774, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

14.3 g of 1-hydroxy-4-amino-N-[γ-(2,4-di-tert-amylphenoxy)propyl]-2-naphthamide obtained in Step (b) of Synthesis I, 6 g of trichloroacetyl chloride and 3.3 g of triethylamine were added to 300 ml of acetonitrile, and the mixture was refluxed for 4 hours. After conclusion of the reaction, the reaction solution was condensed to 100 ml and water was added thereto. The solution was then extracted with ethyl acetate. After removal of the ethyl acetate by distillation, n-hexane was added to the residue. The solid precipitate was separated by filtration and recrystallized from ethanol to obtain the object compound. Yield: 10 g. Melting point: 190° - 192° C.

후처리

  1. temperaturethe mixture was refluxed for 4 hours
  2. customAfter conclusion of the reaction
  3. additionwas added
  4. extractionThe solution was then extracted with ethyl acetate
  5. customAfter removal of the ethyl acetate
  6. distillationby distillation, n-hexane
  7. additionwas added to the residue
  8. customThe solid precipitate was separated by filtration
  9. customrecrystallized from ethanol
  10. customto obtain the object compound

출처 및 근거

ORD 기록
ord-cd8db21af4244c56ba69da2b769a7398
출처 데이터셋
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04083721

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