2-Chloroethylamine hydrochloride → HCID 10268315、化合物

HRID 558262ノート

反応式

HRID 558262 の反応式
[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]

参加物

3

反応物 2

HCID 97937372-Chloroethylamine hydrochlorideHCID 9878953HCID 9878953、化合物

生成物 1

HCID 10268315HCID 10268315、化合物収率 54.3%

反応条件

温度
150 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-3787c67a4cec4b3f95049e7107f7c844
出典データセット
uspto-grants-2011_11
特許番号
US08063044B2

反応ノート

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