Water → HCID 69207606、化合物

HRID 898157

反応式

HRID 898157 の反応式
[ClH:1].[Br:2][C:3]1[CH:21]=[CH:20][C:6]([CH2:7][N:8]2[C:12](=[O:13])[C:11]3([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]3)[NH:10][C:9]2=[O:19])=[CH:5][CH:4]=1.[C:22]1([CH:28]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[CH2:29][CH2:30]Br)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[ClH:1].[Br:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[C:12](=[O:13])[C:11]3([CH2:14][CH2:15][N:16]([CH2:30][CH2:29][CH:28]([C:22]4[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=4)[C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)[CH2:17][CH2:18]3)[NH:10][C:9]2=[O:19])=[CH:20][CH:21]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 883331,1'-(3-Bromopropylidene)bisbenzeneHCID 69207577HCID 69207577、化合物

生成物 1

HCID 69207606HCID 69207606、化合物収率 32.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A mixture of 26.2 mg (70 μmol) of 3-(4-bromo-benzyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione hydrochloride, 21.4 mg (70 μmol) of 3,3-diphenylpropyl bromide and 29 mg (210 μmol) of potassium carbonate in 1 mL of anhydrous DMF was heated overnight at 60° C. After cooling to room temperature, 0.5 mL of water was added and the solution was extracted with DCM (2×2 mL). The crude material was purified by semi-preparative HPLC (method A) yielding 12.8 mg (32.1%) of Compound 3 as a white solid.

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionthe solution was extracted with DCM (2×2 mL)
  3. customThe crude material was purified by semi-preparative HPLC (method A)

出典と根拠

ORDレコード
ord-a6288280573245c68b10df567eb51a5b
出典データセット
uspto-grants-2008_04
特許番号
US07351713B2

関連ノート

読み込み中…