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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2,2'-Bipyridine → 2-Trifluoromethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

HRID 2237449
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HRID 2237449 반응식
C(O[C:4](=O)[CH2:5][N:6]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:7][CH2:8][C:9]1[S:10][CH:11]=[CH:12][CH:13]=1)C.N1C=CC=CC=1C1C=CC=CN=1.[F-].[K+].C[Si]([C:38]([F:41])([F:40])[F:39])(C)C>CN(C=O)C.[Cu]I.CN1C(=O)CCC1>[CH2:17]([O:16][C:14]([N:6]1[CH2:5][CH2:4][C:13]2[CH:12]=[C:11]([C:38]([F:41])([F:40])[F:39])[S:10][C:9]=2[CH2:8][CH2:7]1)=[O:15])[CH3:18]
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참가 물질

8

반응물 4

HCID 14742,2'-BipyridineHCID 522689Potassium FluorideHCID 552549(Trifluoromethyl)trimethylsilaneHCID 66934051[Ethoxycarbonyl-(2-thiophen-2-yl-ethyl)-amino]acetic acid ethyl ester

생성물 1

HCID 684758472-Trifluoromethyl-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylic acid ethyl ester

시약·촉매·용매 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 6228Dimethylformamide용매
HCID 13387N-methyl-2-pyrrolidone용매

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온도
80 °C

실험 절차

A solution of the product from step a.) (75 mg, 0.21 mmol) in DMF (0.5 ml) and NMP (0.5 ml) was treated with bipyridyl (43 mg, 0.27 mmol), CuI (44 mg, 0.23 mmol), KF (13 mg, 0.23 mmol) and trimethylsilyltrifluoromethane (2.1 ml, 1.05 mmol). The reaction mixture was heated to 80° C. for 3 days. The reaction was cooled and filtered through celite washing with EtOAc (20 ml). The eluent was washed with brine (2×3 ml) and dried (MgSO4) providing the subtitle compound as a brown oil that was used without further purification.

후처리

  1. temperatureThe reaction was cooled
  2. filtrationfiltered
  3. washthrough celite washing with EtOAc (20 ml)
  4. washThe eluent was washed with brine (2×3 ml)
  5. dry with materialdried (MgSO4)

출처 및 근거

ORD 기록
ord-2bdb7c26d0cb4058bb29788725dfe7de
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07718647B2

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