Water → HCID 67319070、化合物

HRID 339728

反応式

HRID 339728 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.Br[CH2:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[O:21][CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][CH2:18][NH:19][C:20](=[O:29])[O:21][CH2:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 254436Benzyl 3-bromopropylcarbamate

生成物 1

HCID 67319070HCID 67319070、化合物収率 73.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-(3-Chlorophenyl)piperazine hydrochloride (5 g, 25.4 mmol), benzyl 3-bromopropylcarbamate (8.3 g, 30.5 mmol) and potassium carbonate (10.5 g, 75.9 mmol) were heated to 80° C. in dimethylformamide (100 ml) for overnight under nitrogen condition. After the reaction complete, the reaction mixture was cooled to room temperature and water was added. The organic layer was extracted with ethyl acetate, and washed with water and brine. After drying with MgSO4, the organic layer was filtered and evaporated under reduced pressure to give the title compound (7.2 g, 73%) as light yellow oil, which was used in the deprotection reaction without further purification.

後処理

  1. extractionThe organic layer was extracted with ethyl acetate
  2. washwashed with water and brine
  3. dry with materialAfter drying with MgSO4
  4. filtrationthe organic layer was filtered
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-e6aa6c02a05147e08425fb3fe3817fda
出典データセット
uspto-grants-2014_11
特許番号
US08895558B2

関連ノート

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