Dimethylformamide → HCID 53433946, 화합물

HRID 388472

반응식

HRID 388472 반응식
[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

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 4432411Diphosphoryl tetrachlorideHCID 13411053HCID 13411053, 화합물

생성물 1

HCID 53433946HCID 53433946, 화합물수율 93%

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9b2fc06614244885b6f6f2cb541a336c
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08377949B2

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