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Dimethylformamide → 2-(5-chloro-2-oxo-1,3-benzoxazol-3(2H)-yl)-N-({5,6-dichloro-1-[2-(methoxymethoxy)ethyl]-1H-benzimidazol-2-yl}methyl)-N-methylacetamide

HRID 1428403
ノート
印刷プレビュー

反応式

HRID 1428403 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]([CH2:16][C:17]3[NH:21][C:20]4[CH:22]=[C:23]([Cl:27])[C:24]([Cl:26])=[CH:25][C:19]=4[N:18]=3)[CH3:15])=[O:13])[C:6]=2[CH:28]=1.CN(C=O)C.C([O-])([O-])=O.[K+].[K+].Br[CH2:41][CH2:42][O:43][CH2:44][O:45][CH3:46]>CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][C:8](=[O:10])[N:7]([CH2:11][C:12]([N:14]([CH2:16][C:17]3[N:18]([CH2:41][CH2:42][O:43][CH2:44][O:45][CH3:46])[C:19]4[CH:25]=[C:24]([Cl:26])[C:23]([Cl:27])=[CH:22][C:20]=4[N:21]=3)[CH3:15])=[O:13])[C:6]=2[CH:28]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 33310511-Bromo-2-(methoxymethoxy)ethaneHCID 1176525702-(5-chloro-2-oxo-1,3-benzoxazol-3 (2H)-yl)-N-[(5,6-dichloro-1H-benzimidazol-2-yl)methyl]-N-methylacetamide

生成物 1

HCID 1176525882-(5-chloro-2-oxo-1,3-benzoxazol-3(2H)-yl)-N-({5,6-dichloro-1-[2-(methoxymethoxy)ethyl]-1H-benzimidazol-2-yl}methyl)-N-methylacetamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

To a mixture of 2-(5-chloro-2-oxo-1,3-benzoxazol-3(2H)-yl)-N-[(5,6-dichloro-1H-benzimidazol-2-yl)methyl]-N-methylacetamide (150 mg) and DMF (4.5 mL) were added K2CO3 (94 mg) and 1-bromo-2-(methoxymethoxy)ethane (80 μL), followed by heating and stirring at 70° C. for 5 hours. The reaction mixture was cooled to room temperature and then diluted with EtOAc. The organic layer was washed with water and brine in this order, dried over MgSO4, and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: Hex/EtOAc=50/50-0/100) to obtain 2-(5-chloro-2-oxo-1,3-benzoxazol-3(2H)-yl)-N-({5,6-dichloro-1-[2-(methoxymethoxy)ethyl]-1H-benzimidazol-2-yl}methyl)-N-methylacetamide (110 mg).

後処理

  1. temperatureby heating
  2. temperatureThe reaction mixture was cooled to room temperature
  3. washThe organic layer was washed with water and brine in this order
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluent: Hex/EtOAc=50/50-0/100)

出典と根拠

ORDレコード
ord-554500ec518845d29f0d8a6299990982
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937087B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート