Hydrochloric Acid → HCID 67972354、化合物

HRID 331402ノート

反応式

HRID 331402 の反応式
C(OC([N:8]1[CH2:13][CH:12]=[C:11]([C:14]2[C:19]3[CH:20]=[CH:21][O:22][C:18]=3[C:17]([F:23])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:24]>ClCCl>[ClH:24].[F:23][C:17]1[C:18]2[O:22][CH:21]=[CH:20][C:19]=2[C:14]([C:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH:10]=2)=[CH:15][CH:16]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67972151HCID 67972151、化合物

生成物 1

HCID 67972354HCID 67972354、化合物収率 90.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred solution of 4-(7-fluoro-benzofuran-4-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (0.97 g, 3.06 mmol) in dichloromethane (23 ml) was added at room temperature hydrochloric acid solution (4M in dioxane, 11.5 ml, 45.8 mmol) and the reaction mixture was allowed to stir for 1.5 h. The reaction mixture was evaporated, the residue triturated with diethyl ether (50 ml) and MeOH (1 ml), the precipitate was collected by filtration, washed with diethyl ether and dried to yield 4-(7-fluoro-benzofuran-4-yl)-1,2,3,6-tetrahydro-pyridine hydrochloride as light yellow solid (0.7 g, 90%), MS (ISP) m/z=218.2 [(M+H)+], mp 202° C.

後処理

  1. customThe reaction mixture was evaporated
  2. customthe residue triturated with diethyl ether (50 ml) and MeOH (1 ml)
  3. filtrationthe precipitate was collected by filtration
  4. washwashed with diethyl ether
  5. customdried

出典と根拠

ORDレコード
ord-7a85168600c54b748b4af98cbd512ab5
出典データセット
uspto-grants-2014_11
特許番号
US08877778B2

反応ノート

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