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Hydrochloric Acid → HCID 178478712、化合物

HRID 331400
ノート
印刷プレビュー

反応式

HRID 331400 の反応式
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]2[C:22]2[CH:23]=[CH:24][O:25][C:26]3[C:30]=2[CH:29]=[CH:28][CH:27]=3)[CH2:10][CH2:9]1)(C)(C)C.[ClH:32]>ClCCl>[ClH:32].[ClH:32].[O:25]1[C:26]2=[CH:27][CH:28]=[CH:29][C:30]2=[C:22]([CH:17]2[CH2:18][CH2:19][CH2:20][CH2:21][N:16]2[CH2:15][CH2:14][C@H:11]2[CH2:10][CH2:9][C@H:8]([NH2:7])[CH2:13][CH2:12]2)[CH:23]=[CH:24]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178453895HCID 178453895、化合物

生成物 1

HCID 178478712HCID 178478712、化合物収率 99%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of trans-{4-[2-(4-benzofuran-4-yl-piperidin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester (0.62 g, 1.24 mmol) in dichloromethane (9 ml) was added at room temperature hydrochloric acid solution (4M in dioxane, 4.63 ml, 18.5 mmol) and the mixture was allowed to stir for 2 h, the solvent was evaporated, MeOH (20 ml) and diethyl ether (40 ml) were added and the mixture was allowed to stir for 30 min at room temperature. The precipitate was collected by filtration, washed with diethyl ether and dried to yield the title compound as a white solid (0.49 g, 99%), MS (ISP) m/z=327.4 [(M+H)+], mp 239° C.

後処理

  1. customthe solvent was evaporated
  2. additionMeOH (20 ml) and diethyl ether (40 ml) were added
  3. stirringto stir for 30 min at room temperature
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with diethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-a1b5d5b8c4d24e99b33ec66008035425
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

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