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Acetyl chloride → HCID 58466519、化合物

HRID 1968881
ノート
印刷プレビュー

反応式

HRID 1968881 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]([CH2:20][C@@H:21]([NH:26]C(=O)OC(C)(C)C)[C@@H:22]([CH3:25])[CH2:23][CH3:24])[C:9]([C@@H:11]2[CH2:13][C@H:12]2[C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH:40]1([CH2:44]Br)[CH2:43][CH2:42][CH2:41]1.C(Cl)(=O)C>CO.CN(C=O)C>[NH2:26][C@@H:21]([C@@H:22]([CH3:25])[CH2:23][CH3:24])[CH2:20][N:8]([C:5]1[CH:4]=[CH:3][C:2]([O:1][CH2:44][CH:40]2[CH2:43][CH2:42][CH2:41]2)=[CH:7][CH:6]=1)[C:9]([C@@H:11]1[CH2:13][C@H:12]1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][N:15]=1)=[O:10]
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 4

HCID 6367Acetyl chlorideHCID 11430Potassium CarbonateHCID 2734658(Bromomethyl)cyclobutaneHCID 86658430HCID 86658430、化合物

生成物 1

HCID 58466519HCID 58466519、化合物収率 88.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 6228
Dimethylformamide
溶媒

反応条件

温度
70 °C

実験手順

A mixture of tert-butyl (2S,3S)-1-((1R,2R)—N-(4-hydroxyphenyl)-2-(pyridin-2-yl)cyclopropanecarboxamido)-3-methylpentan-2-ylcarbamate (69 mg, 0.15 mmol), potassium carbonate (63 mg, 0.46 mmol) and DMF (3 mL) was treated with cyclobutylmethyl bromide (21 μL, 0.18 mmol). The resulting reaction mixture was maintained at 70° C. with vigorous stirring overnight. The mixture was allowed to cool to room temperature, then partitioned between H2O (30 mL) and diethyl ether (20 mL). The layers were separated and the aqueous layer was extracted with diethyl ether (2×20 mL). Combined organics were washed with H2O (30 mL) and brine (30 mL), then dried over Na2SO4, filtered and concentrated under reduced pressure to afford a residue that was purified by column chromatography on silica gel (eluting with 30% ethyl acetate in hexanes) to afford an oil that was dissolved in methanol (2 mL) and cooled to 0° C. The cold solution was then treated dropwise with acetyl chloride (290 μL, 4.0 mmol), and then maintained at room temperature overnight. The reaction was concentrated to dryness to afford (1R,2R)-2-pyridin-2-yl-cyclopropanecarboxylic acid ((2S,3S)-2-amino-3-methyl-pentyl)-(4-cyclobutylmethoxy-phenyl)-amide (56 mg, 88% yield) as a white solid: 1H NMR (400 MHz, MeOD) δ 8.61 (d, J=5.3 Hz, 1H), 8.34 (t, J=8.3 Hz, 1H), 7.79 (t, J=6.7 Hz, 1H), 7.54 (d, J=8.3 Hz, 1H), 7.37 (d, J=8.6 Hz, 2H), 6.99 (d, J=8.3 Hz, 2H), 4.28 (dd, J=14.9, 8.8 Hz, 1H), 3.94 (d, J=6.6 Hz, 2H), 3.69 (dd, J=14.9, 2.8 Hz, 1H), 3.34-3.39 (m, 1H), 2.86-2.96 (m, 1H), 2.77 (dt, J=14.6, 7.2 Hz, 1H), 2.08-2.21 (m, 3H), 1.85-2.02 (m, 5H), 1.73-1.84 (m, 1H), 1.67 (dt, J=8.8, 5.5 Hz, 1H), 1.33-1.46 (m, 1H), 1.17-1.30 (m, 1H), 0.98 (d, J=6.8 Hz, 3H), 0.87 (t, J=7.5 Hz, 3H); LRMS (ESI) m/e 422.3 [(M+H)+, calcd for C26H36N3O2 422.3].

後処理

  1. customThe resulting reaction mixture
  2. temperatureto cool to room temperature
  3. custompartitioned between H2O (30 mL) and diethyl ether (20 mL)
  4. customThe layers were separated
  5. extractionthe aqueous layer was extracted with diethyl ether (2×20 mL)
  6. washCombined organics were washed with H2O (30 mL) and brine (30 mL)
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customto afford a residue that
  11. customwas purified by column chromatography on silica gel (eluting with 30% ethyl acetate in hexanes)
  12. customto afford an oil that
  13. temperaturecooled to 0° C
  14. temperaturemaintained at room temperature overnight
  15. concentrationThe reaction was concentrated to dryness

出典と根拠

ORDレコード
ord-44abbca178b04d0bbe399bf9e58aee92
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08426414B2

反応ノート

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