Hydrochloric Acid → HCID 178479251、化合物

HRID 1909359ノート

反応式

HRID 1909359 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][CH:19]([C:22]3[C:30]4[O:29][CH2:28][O:27][C:26]=4[CH:25]=[CH:24][CH:23]=3)[CH2:18][CH2:17]2)[CH2:10][CH2:9]1)(C)(C)C.[ClH:32]>ClCCl>[ClH:32].[O:27]1[C:26]2[CH:25]=[CH:24][CH:23]=[C:22]([CH:19]3[CH2:20][CH2:21][N:16]([CH2:15][CH2:14][C@H:11]4[CH2:10][CH2:9][C@H:8]([NH2:7])[CH2:13][CH2:12]4)[CH2:17][CH2:18]3)[C:30]=2[O:29][CH2:28]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178453890HCID 178453890、化合物

生成物 1

HCID 178479251HCID 178479251、化合物収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of trans-{4-[2-(4-Benzo[1,3]dioxol-4-yl-piperidin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester (1.06 g, 2.46 mmol,) in dichloromethane (15 ml) was added at room temperature hydrochloric acid solution (4M in dioxane, 6.15 ml, 24.6 mmol,) and the mixture was allowed to stir for 4 h, the solvent was evaporated, diisopropyl ether (15 ml) were added and the mixture was allowed to stir for 10 min at room temperature. The precipitate was collected by filtration, washed with diisopropyl ether and dried to yield the title compound as a white solid (0.954, 100%), MS m/z=330.23 [(M)+].

後処理

  1. customthe solvent was evaporated
  2. additiondiisopropyl ether (15 ml) were added
  3. stirringto stir for 10 min at room temperature
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with diisopropyl ether
  6. customdried

出典と根拠

ORDレコード
ord-9d44c3033fdc4780b4d8bf4a8e5997f7
出典データセット
uspto-grants-2013_12
特許番号
US08598357B2

反応ノート

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