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Triethylamine → HCID 178504610, 화합물

HRID 1700399
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HRID 1700399 반응식
[NH2:1][C:2]1[N:6]([C:7]2[C:12](Cl)=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19]#[N:20])[C:3]=1[S:21]([CH3:23])=[O:22].[ClH:24].[NH2:25][OH:26].C(N(CC)CC)C>CO>[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:24])=[CH:11][C:10]([C:14]([F:15])([F:17])[F:16])=[CH:9][C:8]=2[Cl:18])[N:5]=[C:4]([C:19](=[NH:20])[NH:25][OH:26])[C:3]=1[S:21]([CH3:23])=[O:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 108618955-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-methylsulfinylpyrazole

생성물 1

HCID 178504610HCID 178504610, 화합물수율 74.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-methylsulfinylpyrazole (20 g) in methanol (120 ml) was added hydroxylamine hydrochloride (3.99 g), followed by addition of triethylamine (8.0 ml). The mixture was stirred at room temperature overnight then evaporated. The residue was partitioned between water and ethyl acetate. The organic layer was washed with water, followed by wash with brine. The organic layer was dried over anhydrous sodium sulfate. The solution was concentrated by evaporation of solvent. A precipitate was formed and collected by filtration. The solid was washed with small amount of ethyl acetate to give Compound 44 (16.1 g), m.p. 225-226° C.

후처리

  1. customthen evaporated
  2. customThe residue was partitioned between water and ethyl acetate
  3. washThe organic layer was washed with water
  4. washby wash with brine
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationThe solution was concentrated by evaporation of solvent
  7. customA precipitate was formed
  8. filtrationcollected by filtration
  9. washThe solid was washed with small amount of ethyl acetate

출처 및 근거

ORD 기록
ord-18c6a6b695e642318bedcb47fb142ce6
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06350771B1

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