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Potassium Carbonate → Tert-butyl [2-[2-[4-(diphenylmethoxy)-1-piperidinyl]ethyl]-2,3-dihydro-2,4,6,7-tetramethylbenzofuran-5-yl]carbamate

HRID 565665
ノート
印刷プレビュー

反応式

HRID 565665 の反応式
Br[CH2:2][CH2:3][C:4]1([CH3:24])[CH2:8][C:7]2[C:9]([CH3:23])=[C:10]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:11]([CH3:14])=[C:12]([CH3:13])[C:6]=2[O:5]1.[C:25]1([CH:31]([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[O:32][CH:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.O>[C:39]1([CH:31]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[O:32][CH:33]2[CH2:38][CH2:37][N:36]([CH2:2][CH2:3][C:4]3([CH3:24])[CH2:8][C:7]4[C:9]([CH3:23])=[C:10]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])[C:11]([CH3:14])=[C:12]([CH3:13])[C:6]=4[O:5]3)[CH2:35][CH2:34]2)[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=1
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 11430Potassium CarbonateHCID 30175844-BenzhydryloxypiperidineHCID 54438432Tert-butyl [2-(2-bromoethyl)-2,3-dihydro-2,4,6,7-tetramethylbenzofuran-5-yl]carbamate

生成物 1

HCID 53977860Tert-butyl [2-[2-[4-(diphenylmethoxy)-1-piperidinyl]ethyl]-2,3-dihydro-2,4,6,7-tetramethylbenzofuran-5-yl]carbamate収率 92%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A suspension of tert-butyl [2-(2-bromoethyl)-2,3-dihydro-2,4,6,7-tetramethylbenzofuran-5-yl]carbamate (1.2 g), 4-(diphenylmethoxy)piperidine (0.85 g), and potassium carbonate (0.44 g) in N,N-dimethylformamide (20 mL) was stirred at 60° C. for 15 hours. This reaction mixture was diluted with water and extracted with ethyl acetate. The extract was washed with saturated aqueous NaCl, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/methanol=98:2 to 95:5) to provide 1.6 g of the title compound. Yield 92%.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with saturated aqueous NaCl
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/methanol=98:2 to 95:5)

出典と根拠

ORDレコード
ord-c84db3e3158b48c6994c1892346494d0
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06172085B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート