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Ammonia → HCID 57619474, 화합물

HRID 1256849
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HRID 1256849 반응식
[C:1]([O:5][C:6](=[O:24])[N:7]([C:16]1[CH:21]=[CH:20][C:19](Br)=[C:18]([F:23])[N:17]=1)[CH2:8][C:9]1[CH:10]=[N:11][CH:12]=[C:13]([F:15])[CH:14]=1)([CH3:4])([CH3:3])[CH3:2].C([Mg]Cl)(C)C.C([Cu])#N.C(OC([N:40]1[C:44]2=[N:45][CH:46]=[C:47]([C:49]#[N:50])[CH:48]=[C:43]2[C:42]([CH2:51]Cl)=[CH:41]1)=O)(C)(C)C.N>O1CCCC1>[C:1]([O:5][C:6](=[O:24])[N:7]([C:16]1[CH:21]=[CH:20][C:19]([CH2:51][C:42]2[C:43]3[C:44](=[N:45][CH:46]=[C:47]([C:49]#[N:50])[CH:48]=3)[NH:40][CH:41]=2)=[C:18]([F:23])[N:17]=1)[CH2:8][C:9]1[CH:10]=[N:11][CH:12]=[C:13]([F:15])[CH:14]=1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

7

반응물 5

HCID 222AmmoniaHCID 57619177HCID 57619177, 화합물HCID 57619358HCID 57619358, 화합물HCID 178418546HCID 178418546, 화합물HCID 178418918HCID 178418918, 화합물

생성물 1

HCID 57619474HCID 57619474, 화합물수율 94.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

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온도
5 °C

실험 절차

To (5-bromo-6-fluoro-pyridin-2-yl)-(5-fluoro-pyridin-3-ylmethyl)-carbamic acid tert-butyl ester (631, 0.600 g, 1.50 mmol, prepared as described in Example 60) in tetrahydrofuran (10.0 mL) at −25° C. under an atmosphere of nitrogen, was added a solution of isopropylmagnesium chloride (2.0 M in tetrahydrofuran, 0.730 mL). The reaction was allowed to warm to 5° C. over 1 hour. The reaction was cooled to −35° C., followed by addition of a solution of CuCN.2LiCl (0.65 M in tetrahydrofuran, 2.4 mL). After 5 minutes, 3-chloromethyl-5-cyano-pyrrolo[2,3-b]pyridine-1-carboxylic acid tert-butyl ester (635, 0.086 g, 0.29 mmol) in tetrahydrofuran (4.0 mL) was added to the reaction. The reaction was allowed to warm to room temperature over 1 hour, then poured into a diluted ammonia solution, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated and purified by silica gel column chromatography eluting with 20% to 100% ethyl acetate in hexane to give the desired compound (636, 0.13 g, 92%). MS (ESI) [M+H+]+=477.4.

후처리

  1. temperatureThe reaction was cooled to −35° C.
  2. temperatureto warm to room temperature over 1 hour
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated
  7. custompurified by silica gel column chromatography
  8. washeluting with 20% to 100% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-e766c36b4c904c39acbb570e88891ee8
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08461169B2

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