Hydrochloric Acid → HCID 15952779, 화합물

HRID 1927323노트

반응식

HRID 1927323 반응식
[N:1]([C:4]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([C:12]([F:15])([F:14])[F:13])[CH:5]=1)=[C:2]=[S:3].[CH3:16][C:17]([NH:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([CH3:20])[C:18]#N.C[OH:29].Cl>CN(C=O)C.O>[C:22]1([N:21]2[C:17]([CH3:16])([CH3:20])[C:18](=[O:29])[N:1]([C:4]3[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([C:12]([F:13])([F:15])[F:14])[CH:5]=3)[C:2]2=[S:3])[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 751282-Anilino-2-methylpropiononitrileHCID 116155404-Isothiocyanato-2-(trifluoromethyl)benzonitrile

생성물 1

HCID 15952779HCID 15952779, 화합물수율 71%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 1a (0.274 g, 1.2 mmol) and 6a (0.160 g, 1 mmol) in dry DMF (0.2 ml) was stirred for 48 h. To this mixture were added methanol (10 ml) and 2N HCl (3 ml). The second mixture was refluxed for 6 h. After being cooled to room temperature, the reaction mixture was poured into cold water (20 ml) and extracted with ethyl acetate (20 ml). The organic layer was dried over MgSO4, concentrated and chromatographed (dichloromethane) to yield 4-[3-phenyl-4,4-dimethyl-5-oxo-2-thioxoimidazolidin-1-yl]-2-trifluoromethylbenzonitrile, 6b, [RD10] (0.276 g, 0.71 mmol, 71%) as a white powder.

후처리

  1. temperatureThe second mixture was refluxed for 6 h
  2. extractionextracted with ethyl acetate (20 ml)
  3. dry with materialThe organic layer was dried over MgSO4
  4. concentrationconcentrated
  5. customchromatographed (dichloromethane)

출처 및 근거

ORD 기록
ord-16f5838901704cec9960ba67f8e0aa68
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183274B2

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