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alpha-Bromo-o-fluorotoluene → 1-(tert-Butoxycarbonyl)-4-(2-fluorobenzyl)piperidine-4-carboxylic acid

HRID 730198
ノート
印刷プレビュー

反応式

HRID 730198 の反応式
C([N-]C(C)C)(C)C.[Li+].[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][CH:19]([C:22]([OH:24])=[O:23])[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:11])[CH3:10].[F:25][C:26]1[CH:33]=[CH:32][CH:31]=[CH:30][C:27]=1[CH2:28]Br>O1CCCC1>[C:9]([O:13][C:14]([N:16]1[CH2:21][CH2:20][C:19]([CH2:28][C:27]2[CH:30]=[CH:31][CH:32]=[CH:33][C:26]=2[F:25])([C:22]([OH:24])=[O:23])[CH2:18][CH2:17]1)=[O:15])([CH3:12])([CH3:10])[CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 67968alpha-Bromo-o-fluorotolueneHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 2724682Lithium diisopropylamide

生成物 1

HCID 236005311-(tert-Butoxycarbonyl)-4-(2-fluorobenzyl)piperidine-4-carboxylic acid収率 22%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium diisopropylamide (10.9 mmol, 2M tetrahydrofuran) was added to a solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (1.00 g, 4.36 mmol) in tetrahydrofuran (25 mL) at 0° C. After 1.5 h 2-fluorobenzyl bromide (0.788 mL, 6.54 mmol) was added, the reaction mixture was allowed to warm to room temperature and stirred overnight. The reaction was quenched with the addition of water (10 mL) followed by 1M hydrochloric acid (10 mL). The aqueous layer was extracted with ethyl acetate (3×50 mL), the organic layers collected, concentrated under reduced pressure and crude product purified by column chromatography to give 0.330 g, (22 %) of 4-(2-fluoro-benzyl)-piperidine-1,4-dicarboxylic acid mono-tert-butyl ester. 1H-NMR (CD3Cl3, 300 MHz) δ 7.11-7.00 (m, 5H), 4.00 (br., 2H), 2.92 (s, 2H), 2.90 (br., 2H), 2.05 (br., 2H), 1.46 (br., 2H), 1.44 (s, 9H).

後処理

  1. customThe reaction was quenched with the addition of water (10 mL)
  2. extractionThe aqueous layer was extracted with ethyl acetate (3×50 mL)
  3. customthe organic layers collected
  4. concentrationconcentrated under reduced pressure and crude product
  5. custompurified by column chromatography

出典と根拠

ORDレコード
ord-f08888305c91470f8eac81c836f8dbe6
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07582654B2

反応ノート

読み込み中…

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