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Bromine → 3-(2-Bromo-5-morpholinophenoxy)pyridin-2-amine

HRID 1806141
ノート
印刷プレビュー

反応式

HRID 1806141 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[C:9]([CH:18]=[CH:19][CH:20]=2)[O:10][C:11]2[C:12]([NH2:17])=[N:13][CH:14]=[CH:15][CH:16]=2)[CH2:3][CH2:2]1.[Br:21]Br>C(O)(=O)C>[Br:21][C:18]1[CH:19]=[CH:20][C:7]([N:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)=[CH:8][C:9]=1[O:10][C:11]1[C:12]([NH2:17])=[N:13][CH:14]=[CH:15][CH:16]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24408BromineHCID 669950653-(3-Morpholinophenoxy)pyridin-2-amine

生成物 1

HCID 669953443-(2-Bromo-5-morpholinophenoxy)pyridin-2-amine収率 77.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

In a 250 mL round-bottom flask, 3-(3-morpholinophenoxy)pyridin-2-amine (0.720 g, 2.654 mmol) was dissolved in mL of acetic acid and Bromine (2.654 mL, 2.654 mmol) (1M in AcOH) was added slowly. After agitating for 1 hour the mixture was evaporated and the residue was distributed between dichloromethane and sodium bicarbonate solution. The organic phase was separated and evaporated. The residue was purified by column chromatography on silica gel, eluted with 1-3% methanol/dichloromethane to give the title compound (0.72 g, 77%) as white solid.

後処理

  1. additionwas added slowly
  2. customwas evaporated
  3. customThe organic phase was separated
  4. customevaporated
  5. customThe residue was purified by column chromatography on silica gel
  6. washeluted with 1-3% methanol/dichloromethane

出典と根拠

ORDレコード
ord-10455246271b41279d4b568d2cb33064
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354540B2

反応ノート

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