1,1,1-Trifluoro-2,4-pentanedione → HCID 11667432, 화합물

HRID 133511노트

반응식

HRID 133511 반응식
[NH2:1][C:2]1[S:3][C:4]([CH3:16])=[C:5]([CH3:15])[C:6]=1[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O.[F:17][C:18]([F:26])([F:25])[C:19](=[O:24])[CH2:20][C:21](=O)[CH3:22]>C(O)(=O)C.S(=O)(=O)(O)O>[F:17][C:18]([F:26])([F:25])[C:19]([C:20]1[C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:6]2[C:5]([CH3:15])=[C:4]([CH3:16])[S:3][C:2]2=[N:1][C:21]=1[CH3:22])=[O:24]

참가 물질

5

반응물 2

HCID 739431,1,1-Trifluoro-2,4-pentanedioneHCID 615540(2-Amino-4,5-dimethylthiophen-3-yl)(phenyl)methanone

생성물 1

HCID 11667432HCID 11667432, 화합물수율 11%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

To a stirred solution of 50 mg (0.22 mmol) (2-Amino-4,5-dimethyl-thiophen-3-yl)-phenyl-methanone (the preparation of which is described in example 15) in 2 ml acetic acid was added 0.03 ml (0.22 mmol) of 1,1,1-trifluoro-pentane-2,4-dione and one drop of sulfuric acid. The mixture was then stirred at 100° C. for 10 minutes in a microwave and then concentrated in vacuo. Preparative HPLC (30% CH3CN/H20) afforded 8 mg (11%) 2,2,2-trifluoro-1-(2,3,6-trimethyl-4-phenyl-thieno[2,3-b]pyridine-5-yl)-ethanone as an orange solid. ES-MS m/e (%): 350 (M+H+, 100).

후처리

  1. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-952053e23f5d44be86ddbcc69666c2fd
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07390903B2

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