Methanol → HCID 58503866, 화합물

HRID 623810

반응식

HRID 623810 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 58503866HCID 58503866, 화합물

시약·촉매·용매 1

HCID 84541-Methylpyrrolidine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c1d72bb1dd7348c385f766be105920f5
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09303000B2

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