Methanol → HCID 58503866、化合物

HRID 623810

反応式

HRID 623810 の反応式
[H-].[Na+].CO.[Cl:5][C:6]1[CH:7]=[C:8]([CH:11]=[C:12](Cl)[N:13]=1)[C:9]#[N:10].C[CH2:16][O:17]C(C)=O.CCCCCC>CN1CCCC1>[Cl:5][C:6]1[CH:7]=[C:8]([CH:11]=[C:12]([O:17][CH3:16])[N:13]=1)[C:9]#[N:10]

参加物

6

反応物 4

HCID 887MethanolHCID 24758Sodium hydrideHCID 7359062,6-DichloroisonicotinonitrileHCID 21226206Ethyl acetate hexane

生成物 1

HCID 58503866HCID 58503866、化合物

試薬・触媒・溶媒 1

HCID 84541-Methylpyrrolidine溶媒

実験手順

In a 25-mL, 3N round-bottomed flask equipped with thermometer pocket fitted with an nitrogen inlet and a rubber septum, NaH (0.112 g, 1.0 eq.), methanol (0.11 mL, 1.0 eq.), suspended in N-methylpyrrolidine (5 mL). The reaction mixture was stir at 25-30 C for 30 minutes. To this reaction mixture 2,6-dichloroisonicotinonitrile was added at 0-5 C. The progress of the reaction was followed by TLC analysis on silica gel with 10% EtOAc-hexane as mobile phase which shows that starting material was consumed after 2 hours staring at 0-5 C. Reaction was quenched by water, precipitate was observed that was filter by filter paper and wash with hexane to give required compound (0.51 g, crude). Reaction was stirred for 20 min with water solid was separated and compound was collected by filtration on a Buchner funnel and washed with of hexane (30 mL); Yield: 0.51 g crude 2-chloro-6-methoxyisonicotinonitrile.

後処理

  1. customIn a 25-mL, 3N round-bottomed flask equipped with thermometer pocket
  2. customfitted with an nitrogen inlet
  3. customwas consumed after 2 hours
  4. customReaction
  5. customwas quenched by water, precipitate
  6. filtrationthat was filter
  7. filtrationby filter paper
  8. washwash with hexane

出典と根拠

ORDレコード
ord-c1d72bb1dd7348c385f766be105920f5
出典データセット
uspto-grants-2016_04
特許番号
US09303000B2

関連ノート

読み込み中…