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Ammonia → HCID 57619474、化合物

HRID 1256849
ノート
印刷プレビュー

反応式

HRID 1256849 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 222AmmoniaHCID 57619177HCID 57619177、化合物HCID 57619358HCID 57619358、化合物HCID 178418546HCID 178418546、化合物HCID 178418918HCID 178418918、化合物

生成物 1

HCID 57619474HCID 57619474、化合物収率 94.1%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
3 回

反応条件

温度
5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e766c36b4c904c39acbb570e88891ee8
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461169B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート