Morpholine → Ammonia

HRID 385947ノート

反応式

HRID 385947 の反応式
Br[CH2:2][C:3]1[C:4]([CH3:10])=[N:5][C:6]([Cl:9])=[CH:7][CH:8]=1.[NH:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1.CCN(C(C)C)C(C)C>C(Cl)Cl.O>[NH3:5].[Cl:9][C:6]1[N:5]=[C:4]([CH3:10])[C:3]([CH2:2][N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)=[CH:8][CH:7]=1

参加物

7

反応物 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 595261743-(Bromomethyl)-6-chloro-2-methylpyridine

生成物 2

HCID 222AmmoniaHCID 513419534-[(6-Chloro-2-methylpyridin-3-yl)methyl]morpholine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

3-(Bromomethyl)-6-chloro-2-methylpyridine (500 mg, 2.27 mmol) was taken up in CH2Cl2 (5.0 mL) and morpholine (257 μL, 2.95 mmol) and DIEA (594 μL, 3.40 mmol) were added. After stirring at room temperature overnight, the reaction was diluted with water and extracted with CH2Cl2 (2×). The combined organic layers were dried over MgSO4, filtered, and evaporated. Flash chromatography (0-10% MeOH (w/2 M NH3)/CH2Cl2) provided the title compound as a colorless oil.

後処理

  1. extractionextracted with CH2Cl2 (2×)
  2. dry with materialThe combined organic layers were dried over MgSO4
  3. filtrationfiltered
  4. customevaporated

出典と根拠

ORDレコード
ord-d3b4e8cd363f4bcba022ccba1d4517a5
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

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