Water → 4-(1-ethyl-1H-benzoimidazol-2-ylmethoxy)-2-fluoro-5-methoxy-benzaldehyde

HRID 253475ノート

反応式

HRID 253475 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[CH2:10][O:11][C:12]1[C:19]([O:20][CH3:21])=[CH:18][C:15]([CH:16]=[O:17])=[C:14]([F:22])[CH:13]=1.[H-].[Na+].Br[CH2:26][CH3:27].O>CN(C)C(=O)C>[CH2:26]([N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[CH2:10][O:11][C:12]1[C:19]([O:20][CH3:21])=[CH:18][C:15]([CH:16]=[O:17])=[C:14]([F:22])[CH:13]=1)[CH3:27]

参加物

6

反応物 4

HCID 962WaterHCID 6332Ethyl BromideHCID 24758Sodium hydrideHCID 580860204-(1H-benzimidazol-2-ylmethoxy)-2-fluoro-5-methoxy-benzaldehyde

生成物 1

HCID 598038224-(1-ethyl-1H-benzoimidazol-2-ylmethoxy)-2-fluoro-5-methoxy-benzaldehyde収率 89%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of 4-(1H-benzoimidazol-2-ylmethoxy)-2-fluoro-5-methoxy-benzaldehyde (215, 4.0 g, 13 mmol) in N,N-dimethylacetamide (80 mL) was added sodium hydride (60% dispersion in mineral oil, 0.65 g, 16 mmol) portion wise. After the addition was complete, the reaction was stirred for 30 minutes after which bromoethane (1.2 mL, 16 mmol) was added and then allowed to stir for several hours. The reaction mixture was then poured into water (1 L) with stirring and the precipitated solid was filtered, washed with water and dried to give the desired compound (216, 3.8 g, 87% yield).

後処理

  1. additionAfter the addition
  2. additionwas added
  3. stirringwith stirring
  4. filtrationthe precipitated solid was filtered
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-af7fd7be89234770830ee24e89cb90a7
出典データセット
uspto-grants-2011_01
特許番号
US07872018B2

反応ノート

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