Dimethylformamide → HCID 53433946、化合物

HRID 388472

反応式

HRID 388472 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[C:6]([CH3:12])[CH:7]=[C:8]([CH3:11])[CH:9]=2)[CH:4]=[CH:3]1.P(Cl)(Cl)(OP(Cl)(Cl)=O)=O.CN([CH:25]=[O:26])C>>[CH3:1][N:2]1[C:10]2[C:5](=[C:6]([CH3:12])[CH:7]=[C:8]([CH3:11])[CH:9]=2)[C:4]([CH:25]=[O:26])=[CH:3]1

参加物

4

反応物 3

HCID 6228DimethylformamideHCID 4432411Diphosphoryl tetrachlorideHCID 13411053HCID 13411053、化合物

生成物 1

HCID 53433946HCID 53433946、化合物収率 93%

実験手順

A solution of 1,4,6-trimethyl-1H-indole (800 mg, 5 mmol) in DMF (0.9 mL) is cooled to 5° C. under nitrogen. Pyrophosphoryl chloride (1.4 mL, 10 mmol) is then slowly introduced. Upon complete addition the cooling bath is removed and the reaction is allowed to warm to ambient temperature. After a total of 45 minutes, the reaction is recooled to 5° C. and is slowly quenched with 2N NaOH. The pH of the solution is adjusted to 8. The precipitated solid is collected by filtration and is washed with water to afford 1,4,6-Trimethyl-1H-indole-3-carbaldehyde (875 mg, 93%).

後処理

  1. additionUpon complete addition the cooling bath
  2. customis removed
  3. customAfter a total of 45 minutes
  4. customis recooled to 5° C.
  5. customis slowly quenched with 2N NaOH
  6. filtrationThe precipitated solid is collected by filtration
  7. washis washed with water

出典と根拠

ORDレコード
ord-9b2fc06614244885b6f6f2cb541a336c
出典データセット
uspto-grants-2013_02
特許番号
US08377949B2

関連ノート

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