Triethylamine → 2-Fluoro-5-((3-oxo-4,5,6,7-tetrahydroisobenzofuran-1 (3h)-ylidene)methyl)benzonitrile

HRID 1259275노트

반응식

HRID 1259275 반응식
[Br-].C([P+](CCCC)(CCCC)[CH:7]1[C:11]2[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=2[C:9](=[O:16])[O:8]1)CCC.[F:25][C:26]1[CH:33]=[CH:32][C:31]([CH:34]=O)=[CH:30][C:27]=1[C:28]#[N:29].C(N(CC)CC)C>ClCCl>[F:25][C:26]1[CH:33]=[CH:32][C:31]([CH:34]=[C:7]2[C:11]3[CH2:12][CH2:13][CH2:14][CH2:15][C:10]=3[C:9](=[O:16])[O:8]2)=[CH:30][C:27]=1[C:28]#[N:29]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27695822-Fluoro-5-formylbenzonitrileHCID 66966753Tributyl(3-oxo-1,3,4,5,6,7-hexahydro-2-benzofuran-1-yl)phosphonium bromide

생성물 1

HCID 690434422-Fluoro-5-((3-oxo-4,5,6,7-tetrahydroisobenzofuran-1 (3h)-ylidene)methyl)benzonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of EXAMPLE 1B (3.05 g) in dichloromethane (30 mL) was added 2-fluoro-5-formylbenzonitrile (1.08 g) and triethylamine (1.02 mL). The mixture was stirred at ambient temperature for 16 hours and concentrated. The concentrate was partitioned between ethyl acetate and brine. The organic layer was washed with brine and concentrated. The concentrate was purified by flash chromatography on silica gel with 50% ethyl acetate in hexane.

후처리

  1. concentrationconcentrated
  2. customThe concentrate was partitioned between ethyl acetate and brine
  3. washThe organic layer was washed with brine
  4. concentrationconcentrated
  5. customThe concentrate was purified by flash chromatography on silica gel with 50% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-32230feb7b7b4cf195354b33a069cfe9
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466150B2

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