Methylamine → HCID 68532585、化合物

HRID 1967414ノート

反応式

HRID 1967414 の反応式
Cl[C:2](Cl)(Cl)[C:3](Cl)=[O:4].O1CCCC1.[CH2:13]([CH:15]([C:18]1[CH:19]=[C:20]([CH3:23])[NH:21]C=1)[CH2:16][CH3:17])[CH3:14].[CH3:24][NH2:25]>O>[CH2:13]([CH:15]([C:18]1[CH:19]=[C:20]([CH3:23])[NH:21][C:2]=1[C:3]([NH:25][CH3:24])=[O:4])[CH2:16][CH3:17])[CH3:14]

参加物

6

反応物 4

HCID 6329MethylamineHCID 6420Trichloroacetyl chlorideHCID 8028TetrahydrofuranHCID 68530648HCID 68530648、化合物

生成物 1

HCID 68532585HCID 68532585、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

Trichloroacetyl chloride (2.03 mL) was added to the tetrahydrofuran solution (36 mL) of the compound prepared in Example 3 (2.76 g), and the reaction mixture was stirred at 0° C. for an hour. The reaction mixture was dropped to an aqueous solution of 40% methylamine (36 mL) on ice bath, and stirred at room temperature for 30 minutes. Water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate. The organic layer was washed by a saturated aqueous solution of sodium chloride, and dried with anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (high flash-SI, size 3 L (made in Yamazen corporation), n-hexane/ethyl acetate=60/40→35/65) to obtain a title compound (1.55 g) having the following physical data.

後処理

  1. stirringstirred at room temperature for 30 minutes
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. washThe organic layer was washed by a saturated aqueous solution of sodium chloride
  4. dry with materialdried with anhydrous sodium sulfate
  5. concentrationThe organic layer was concentrated under reduced pressure
  6. customThe obtained residue was purified by column chromatography on silica gel (high flash-SI, size 3 L (made in Yamazen corporation), n-hexane/ethyl acetate=60/40→35/65)

出典と根拠

ORDレコード
ord-5be29a2d177442b0a3f11eabf9c6f73a
出典データセット
uspto-grants-2013_04
特許番号
US08420810B2

反応ノート

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