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Cesium carbonate → HCID 86731737、化合物

HRID 1504868
ノート
印刷プレビュー

反応式

HRID 1504868 の反応式
Br[C:2]1[CH:3]=[C:4]([NH:10][C@@H:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C@@H:12]2[NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH:5]=[N:6][C:7]=1[C:8]#[N:9].[NH2:25][C:26]1[N:31]=[C:30]([CH3:32])[C:29]([C:33]#[N:34])=[CH:28][CH:27]=1.C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.C(=O)([O-])[O-].[Cs+].[Cs+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:8]([C:7]1[N:6]=[CH:5][C:4]([NH:10][C@@H:11]2[CH2:16][CH2:15][CH2:14][CH2:13][C@@H:12]2[NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[CH:3][C:2]=1[NH:25][C:26]1[CH:27]=[CH:28][C:29]([C:33]#[N:34])=[C:30]([CH3:32])[N:31]=1)#[N:9]
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

6

反応物 4

HCID 10796Cesium carbonateHCID 27946626-Amino-2-methylpyridine-3-carbonitrileHCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 86716545tert-butyl (1S,2R)-2-(5-bromo-6-cyanopyridin-3-ylamino)cyclohexylcarbamate

生成物 1

HCID 86731737HCID 86731737、化合物

試薬・触媒・溶媒 1

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒

反応条件

温度
100 °C

実験手順

To a flask containing tert-butyl {(1S,2R)-2-[(5-bromo-6-cyanopyridin-3-yl)amino]cyclohexyl}carbamate (PrepEx 1.1) (120 mg, 0.30 mmol), 6-amino-2-methylpyridine-3-carbonitrile (40 mg, 0.30 mmol), 2-dicyclohexylphosphino-2′,4′,6′-triisopropylbiphenyl (29 mg, 0.061 mmol), Pd2(dba)3 (28 mg, 0.031 mmol) and cesium carbonate (198 mg, 0.609 mmol) was added degassed dioxane (3 mL). The reaction mixture was heated to 100° C. overnight. The reaction mixture was cooled to room temperature, diluted with ethyl acetate and water, and the organic layer was separated, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. Purification by chromatography on silica gel (0-40% ethyl acetate/hexanes, linear gradient) afforded tert-butyl [(1S,2R)-2-({6-cyano-5-[(5-cyano-6-methylpyridin-2-yl)amino]pyridin-3-yl}amino)cyclohexyl]carbamate. MS ESI calc'd for C24H30N7O2 [M+H]+ 448. found 448. 1H NMR (500 MHz, DMSO-d6) δ 9.62 (s, 1H), 7.92-7.86 (m, 2H), 7.26 (s, 1H), 6.81 (d, J=8.8 Hz, 1H), 6.64 (d, J=8.5 Hz, 1H), 6.56 (d, J=7.7 Hz, 1), 3.75-3.64 (m, 2H), 2.47 (s, 3H), 1.75-1.42 (m, 8H), 1.26 (s, 9H).

後処理

  1. additionwas added
  2. customdegassed dioxane (3 mL)
  3. temperatureThe reaction mixture was cooled to room temperature
  4. additiondiluted with ethyl acetate and water
  5. customthe organic layer was separated
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customPurification by chromatography on silica gel (0-40% ethyl acetate/hexanes, linear gradient)

出典と根拠

ORDレコード
ord-9e5760f3c6494ffb9e5796e727f82a97
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216173B2

反応ノート

読み込み中…

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