2-Chloroethylamine hydrochloride → HCID 10268315, 화합물

HRID 558262노트

반응식

HRID 558262 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[C:16]([Cl:18])[CH:17]=1)[O:5][C:6]1[C:7]([CH2:13][CH3:14])=[N:8][NH:9][C:10]=1[CH2:11][CH3:12].Cl.Cl[CH2:21][CH2:22][NH2:23]>>[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[C:16]([Cl:18])[CH:17]=1)[O:5][C:6]1[C:10]([CH2:11][CH3:12])=[N:9][N:8]([CH2:21][CH2:22][NH2:23])[C:7]=1[CH2:13][CH3:14]

참가 물질

3

반응물 2

HCID 97937372-Chloroethylamine hydrochlorideHCID 9878953HCID 9878953, 화합물

생성물 1

HCID 10268315HCID 10268315, 화합물수율 54.3%

반응 조건

온도
150 °C

실험 절차

A mixture of the pyrazole (390 mg, 1.37 mmol) of Example 3 and chloroethylamine hydrochloride (238 mg, 2.05 mmol) was stirred and heated at 150° C. for 24 hours. After cooling, the mixture was partitioned between saturated aqueous sodium bicarbonate solution (100 ml) and dichloromethane (2×50 ml). The combined organic layers were washed with brine (30 ml), dried over magnesium sulphate, filtered and concentrated under reduced pressure. The resulting brown oil was purified by flash chromatography on silica gel eluting with dichloromethane:methanol (90:10, by volume) to afford the title compound (244 mg) as a brown oil.

후처리

  1. temperatureAfter cooling
  2. customthe mixture was partitioned between saturated aqueous sodium bicarbonate solution (100 ml) and dichloromethane (2×50 ml)
  3. washThe combined organic layers were washed with brine (30 ml)
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe resulting brown oil was purified by flash chromatography on silica gel eluting with dichloromethane:methanol (90:10, by volume)

출처 및 근거

ORD 기록
ord-3787c67a4cec4b3f95049e7107f7c844
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063044B2

반응 노트

불러오는 중…