(E)-pent-2-enoyl chloride → HCID 56949206、化合物

HRID 333971

反応式

HRID 333971 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[N:6]2[N:15]=[CH:16][CH:17]=[C:5]2[N:4]=1.[C:18](Cl)(=[O:23])/[CH:19]=[CH:20]/[CH2:21][CH3:22]>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N:9]2[CH2:10][CH2:11][N:12]([C:18](=[O:23])/[CH:19]=[CH:20]/[CH2:21][CH3:22])[CH2:13][CH2:14]2)[N:6]2[N:15]=[CH:16][CH:17]=[C:5]2[N:4]=1

参加物

4

反応物 2

HCID 5706546(E)-pent-2-enoyl chlorideHCID 66835729HCID 66835729、化合物

生成物 1

HCID 56949206HCID 56949206、化合物収率 51%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

5-Methoxy-7-piperazin-1-yl-pyrazolo[1,5-a]pyrimidine (23.3 mg, 0.1 mmol) was dissolved in anhydrous dichloromethane (1 ml), TEA (17.4 μl, 1.25 mmol) followed by (E)-pent-2-enoyl chloride (14.8 mg, 0.125 mmol) were added, the mixture was shaken for 10 minutes, diluted with dichloromethane, washed with 10% sodium bicarbonate solution, water and the organic phase was evaporated to dryness under reduced pressure. The residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 16.1 mg of a solid (0.05 mmol, 51%).

後処理

  1. additionwere added
  2. washwashed with 10% sodium bicarbonate solution, water
  3. customthe organic phase was evaporated to dryness under reduced pressure
  4. customThe residue was purified by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)

出典と根拠

ORDレコード
ord-e503c9f02bcb4dc2ac00b64268061954
出典データセット
uspto-grants-2014_11
特許番号
US08883791B2

関連ノート

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