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Bromoacetyl bromide → tert-butyl 4-(2-bromo-N-(4-(trifluoromethyl)phenyl)acetamido)piperidine-1-carboxylate

HRID 1667207
ノート
印刷プレビュー

反応式

HRID 1667207 の反応式
[F:1][C:2]([F:24])([F:23])[C:3]1[CH:8]=[CH:7][C:6]([NH:9][CH:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]2)=[CH:5][CH:4]=1.C(N(C(C)C)C(C)C)C.[Br:34][CH2:35][C:36](Br)=[O:37]>O1CCCC1.C(OCC)(=O)C>[Br:34][CH2:35][C:36]([N:9]([CH:10]1[CH2:11][CH2:12][N:13]([C:16]([O:18][C:19]([CH3:21])([CH3:20])[CH3:22])=[O:17])[CH2:14][CH2:15]1)[C:6]1[CH:5]=[CH:4][C:3]([C:2]([F:1])([F:23])[F:24])=[CH:8][CH:7]=1)=[O:37]
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 3

HCID 61147Bromoacetyl bromideHCID 81531DiisopropylethylamineHCID 220291421-Boc-4-(4-Trifluoromethyl-phenylamino)-piperidine

生成物 1

HCID 67445908tert-butyl 4-(2-bromo-N-(4-(trifluoromethyl)phenyl)acetamido)piperidine-1-carboxylate

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
0 °C

実験手順

A solution of the product of Example 166A (480 mg, 1.39 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.486 mL, 2.79 mmol) in anhydrous tetrahydrofuran (10 mL) was cooled in an ice water bath for 10 minutes followed by the dropwise addition of bromoacetyl bromide (0.146 mL, 1.67 mmol) via syringe. The reaction was stirred for 30 minutes at 0° C., then 1 hour at ambient temperature and 3 hours at reflux. The reaction mixture was cooled to ambient temperature and diluted with ethyl acetate. The organic solution was washed with 1 N aqueous HCl and saturated NaHCO3 solution and brine, dried with Na2SO4, filtered, and concentrated in vacuo. The crude product was chromatographed on silica gel (Analogix® Intelliflash™ 280; SF25-60 g column; 50% ethyl acetate/hexanes) which yielded the title compound. 1H NMR (300 MHz, CDCl3) δ ppm 7.74 (d, J=8.4, 2H), 7.34 (d, J=8.2, 2H), 4.80-4.66 (m, 1H), 4.25-4.04 (m, 2H), 3.49 (s, 2H), 2.79 (t, J=12.4, 2H), 1.87-1.77 (m, 2H), 1.39 (s, 9H), 1.29-1.11 (m, 2H); MS (DCI+) m/z 482/484 (M+NH4)+.

後処理

  1. temperature1 hour at ambient temperature and 3 hours at reflux
  2. temperatureThe reaction mixture was cooled to ambient temperature
  3. washThe organic solution was washed with 1 N aqueous HCl and saturated NaHCO3 solution and brine
  4. dry with materialdried with Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe crude product was chromatographed on silica gel (Analogix® Intelliflash™ 280; SF25-60 g column; 50% ethyl acetate/hexanes) which

出典と根拠

ORDレコード
ord-1aa1cb090210495e9c03da96d3356b9e
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044069B2

反応ノート

読み込み中…

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