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2-Bromopyridine → 5-(1-(pyridin-2-yl)pyrrolidin-2-yl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide

HRID 1473423
ノート
印刷プレビュー

反応式

HRID 1473423 の反応式
COC1C=C(OC)C=CC=1C[N:6]([C:25]1[S:29][N:28]=[CH:27][N:26]=1)[S:7]([C:10]1[CH:19]=[CH:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][C:16]=2[CH:20]2[CH2:24][CH2:23][CH2:22][NH:21]2)[CH:11]=1)(=[O:9])=[O:8].COC(C)(C)C.C(=O)([O-])[O-].[Cs+].[Cs+].Br[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][N:50]=1>CCOC(C)=O.C1(C)C=CC=CC=1>[N:50]1[CH:51]=[CH:52][CH:53]=[CH:54][C:49]=1[N:21]1[CH2:22][CH2:23][CH2:24][CH:20]1[C:16]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:17]=1[CH:18]=[CH:19][C:10]([S:7]([NH:6][C:25]1[S:29][N:28]=[CH:27][N:26]=1)(=[O:9])=[O:8])=[CH:11]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79732-BromopyridineHCID 10796Cesium carbonate2 回HCID 15413tert-Butyl methyl etherHCID 86687400N-(2,4-dimethoxybenzyl)-5-(pyrrolidin-2-yl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide

生成物 1

HCID 715865135-(1-(pyridin-2-yl)pyrrolidin-2-yl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide収率 33.3%

試薬・触媒・溶媒

2
HCID 1140Toluene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A vial was charged with N-(2,4-dimethoxybenzyl)-5-(pyrrolidin-2-yl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide (INTERMEDIATE KK) (34.01 mg, 0.067 mmol), chloro(2-dicyclohexylphosphino-2′,6′-di-1-propoxy-1,1′-biphenyl)[2-(2-aminoethylphenyl)]palladium(II), methyl-t-butylether adduct (Strem Chemical, Newburyport, Mass., 2.72 mg, 3.33 mmol), and cesium carbonate (65.1 mg, 0.200 mmol). The vial was flushed with Ar (g), then toluene (0.3 mL) and 2-bromopyridine (19.05 μl, 0.200 mmol) were added. The vial was sealed and placed in a 100° C. heating bath. After 4 h, an additional portion of catalyst (about 3 mg) was added, and the vial was heated for an additional 16 h. Additional portions of catalyst (6 mg) and cesium carbonate (about 55 mg) were added, and the vial was returned to the heat for 5 h. The mixture was cooled to room temperature, diluted with EtOAc, and filtered through diatomaceous earth. The filtrate was concentrated. The residue was purified by chromatography on silica gel (12-g column, 0 to 10% MeOH/DCM) to give 5-(1-(pyridin-2-yl)pyrrolidin-2-yl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide (9.7 mg, 0.022 mmol, 33.3% yield) as a yellow solid: 1H NMR (400 MHz, DMSO-d6) δ ppm=8.54 (d, J=2.0 Hz, 1H), 8.45 (s, 1H), 8.38 (d, J=9.2 Hz, 1H), 8.12 (d, J=8.2 Hz, 1H), 8.02-7.88 (m, 2H), 7.72 (br. s., 1H), 7.56-7.48 (m, 1H), 7.33 (d, J=6.9 Hz, 1H), 6.79 (t, J=6.4 Hz, 1H), 6.61 (br. s., 1H), 5.91 (d, J=7.8 Hz, 1H), 4.04 (t, J=8.6 Hz, 1H), 3.77-3.62 (m, 1H), 2.71-2.59 (m, 1H), 2.17-2.05 (m, 1H), 2.01-1.84 (m, 2H); m/z (ESI) 438.4 (M+H)+.

後処理

  1. customThe vial was flushed with Ar (g)
  2. customThe vial was sealed
  3. customplaced in a 100° C.
  4. temperatureheating bath
  5. temperaturethe vial was heated for an additional 16 h
  6. temperatureheat for 5 h
  7. filtrationfiltered through diatomaceous earth
  8. concentrationThe filtrate was concentrated
  9. customThe residue was purified by chromatography on silica gel (12-g column, 0 to 10% MeOH/DCM)

出典と根拠

ORDレコード
ord-b0ed7ce9fdbb4393b1ee08f2c3a48e13
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012443B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート