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Triethylamine → HCID 178453895、化合物

HRID 331399
ノート
印刷プレビュー

反応式

HRID 331399 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[C:9](C3CCNCC3)[C:4]=2[CH:3]=[CH:2]1.[C:16]([O:20][C:21](=[O:32])[NH:22][C@H:23]1[CH2:28][CH2:27][C@H:26]([CH2:29][CH:30]=O)[CH2:25][CH2:24]1)([CH3:19])([CH3:18])[CH3:17].C([N:35]([CH2:38][CH3:39])[CH2:36][CH3:37])C.[C:40](=O)(O)[O-].[Na+]>ClCCl>[C:16]([O:20][C:21](=[O:32])[NH:22][C@H:23]1[CH2:28][CH2:27][C@H:26]([CH2:29][CH2:30][N:35]2[CH2:36][CH2:37][CH2:40][CH2:39][CH:38]2[C:7]2[CH:6]=[CH:5][O:1][C:2]3[C:8]=2[CH:9]=[CH:4][CH:3]=3)[CH2:25][CH2:24]1)([CH3:19])([CH3:18])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 679724334-(4-Benzofuranyl)-piperidineHCID 178453924HCID 178453924、化合物

生成物 1

HCID 178453895HCID 178453895、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 4-(4-benzofuranyl)-piperidine (0.3 g, 1.49 mmol) in dichloromethane (8 ml) was added at room temperature commercially available trans-tert-butyl-4-(2-oxoethyl)-cyclohexylcarbamate (1.71 mg, 6.02 mmol) and triethylamine (0.3 g, 0.42 ml, 2.98 mmol) and the solution was allowed to stir for 30 min. Sodium triacetoxyboron hydride (0.57 g, 2.68 mmol) was added step wise and the mixture was allowed to stir for 16 h at room temperature. The solution was poured into saturated sodium bicarbonate solution (20 ml) and extracted with dichloromethane (2×40 ml). The combined organic layers were washed with saturated sodium bicarbonate solution (20 ml), dried (MgSO4) and evaporated. The crude material (0.77 g) was purified by flash chromatography on silica gel (dichloromethane/MeOH 5-10%) to yield trans-{4-[2-(4-benzofuran-4-yl-piperidin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester as a white solid (0.63 g, 99%), MS (ISP) m/z=427.4 [(M+H)+], mp 133° C.

後処理

  1. stirringto stir for 16 h at room temperature
  2. extractionextracted with dichloromethane (2×40 ml)
  3. washThe combined organic layers were washed with saturated sodium bicarbonate solution (20 ml)
  4. dry with materialdried (MgSO4)
  5. customevaporated
  6. customThe crude material (0.77 g) was purified by flash chromatography on silica gel (dichloromethane/MeOH 5-10%)

出典と根拠

ORDレコード
ord-31bb30d1cac142f0aec5f453e9e99bef
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877778B2

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