Water → 3-Chloro-N-[1-(2-chlorophenyl)-2-[1-(2,2,2-trifluoroacetyl)-piperidin-4-ylmethoxy]ethyl]-1H-indole-6-carboxamide

HRID 32427

反応式

HRID 32427 の反応式
[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([NH:13][CH:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[Cl:30])[CH2:15][O:16][CH2:17][CH:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)=[O:12])=[CH:8][CH:9]=2)[NH:4][CH:3]=1.C(N(CC)CC)C.C([O:40][C:41](=O)[C:42]([F:45])([F:44])[F:43])C.O>CO>[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([NH:13][CH:14]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[Cl:30])[CH2:15][O:16][CH2:17][CH:18]3[CH2:23][CH2:22][N:21]([C:41](=[O:40])[C:42]([F:45])([F:44])[F:43])[CH2:20][CH2:19]3)=[O:12])=[CH:8][CH:9]=2)[NH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 9794Ethyl trifluoroacetateHCID 693078883-chloro-N-[1-(2-chlorophenyl)-2-(piperidin-4-ylmethoxy)ethyl]-1H-indole-6-carboxamide

生成物 1

HCID 866036013-Chloro-N-[1-(2-chlorophenyl)-2-[1-(2,2,2-trifluoroacetyl)-piperidin-4-ylmethoxy]ethyl]-1H-indole-6-carboxamide収率 42.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 3-chloro-N-[1-(2-chlorophenyl)-2-(piperidin-4-ylmethoxy)ethyl]-1H-indole-6-carboxamide (600 mg, 1.3 mmol) in 5 mL of methanol was added triethylamine (0.37 mL, 2.7 mmol) and trifluoroacetic acid ethyl ester (0.20 mL, 2.7 mmol). The reaction was allowed to stir at room temperature overnight after which time water was added and the resulting precipitate was isolated by filtration. Purification of the filtrate (SiO2: 10:2:0.5 DCM:hexane:isopropylamine) provided 297 mg (41%) of the title compound.

後処理

  1. additionwas added
  2. customthe resulting precipitate was isolated by filtration
  3. customPurification of the filtrate (SiO2: 10:2:0.5 DCM:hexane:isopropylamine)

出典と根拠

ORDレコード
ord-5e244fec7d16455e9dde4969716cd94a
出典データセット
uspto-grants-2008_09
特許番号
US07427632B2

関連ノート

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