N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide → 4-Iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine

HRID 1348557노트

반응식

HRID 1348557 반응식
[I:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)[N:5]=[CH:4][C:3]=1[NH:15]C(=O)C(C)(C)C>Cl>[I:1][C:2]1[CH:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)[N:5]=[CH:4][C:3]=1[NH2:15]

참가 물질

3

반응물 1

HCID 15887409N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide

생성물 1

HCID 210916424-Iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine수율 92%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
100 °C

실험 절차

A mixture of 2.20 g (5.47 mmol) N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-2,2-dimethyl-propionamide (synthesis described in DE10008042) in 50 ml 3 N hydrochloric acid was stirred for 18 h at 100° C. After cooling to 0° C. the reaction mixture was washed twice with ether (50 ml). The aqueous phase was treated with 50 ml dichloromethane and basified with a 1 M solution of sodium carbonate. The organic phase was separated and the aqueous phase was extracted four times with 50 ml dichloromethane. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 1.60 g (92%) of the title compound as an off-white solid.

후처리

  1. temperatureAfter cooling to 0° C. the reaction mixture
  2. washwas washed twice with ether (50 ml)
  3. additionThe aqueous phase was treated with 50 ml dichloromethane
  4. customThe organic phase was separated
  5. extractionthe aqueous phase was extracted four times with 50 ml dichloromethane
  6. dry with materialThe combined organic layers were dried over sodium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-65ba94ea9e7c4e7bac31fda44fcf68c0
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07211579B2

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