Water → HCID 86685596、化合物

HRID 2200479ノート

反応式

HRID 2200479 の反応式
[Cl:1][C:2]1[C:3]([C:9]#[N:10])=[N:4][CH:5]=[C:6](Cl)[N:7]=1.Cl.[NH2:12][C:13]1([C:17]([NH2:19])=[O:18])[CH2:16][CH2:15][CH2:14]1.CCN(C(C)C)C(C)C.O>CN(C=O)C.CCOC(C)=O>[Cl:1][C:2]1[N:7]=[C:6]([NH:12][C:13]2([C:17]([NH2:19])=[O:18])[CH2:16][CH2:15][CH2:14]2)[CH:5]=[N:4][C:3]=1[C:9]#[N:10]

参加物

7

反応物 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 529877443,5-Dichloropyrazine-2-carbonitrileHCID 717569071-Aminocyclobutane-1-carboxamide hydrochloride

生成物 1

HCID 86685596HCID 86685596、化合物収率 15.2%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3,5-dichloropyrazine-2-carbonitrile (100 mg, 0.574 mmol), 1-aminocyclobutanecarboxamide hydrochloride (108 mg, 0.717 mmol) and DIEA (0.350 mL, 2.01 mmol) in DMF (4 mL) was stirred at room temperature for 70 h. Water and EtOAc were added. Organic phase was separated, washed with 1N HCl, then with 5% NaHCO3, dried over Na2SO4, concentrated in vacuo. The residue was purified by HPLC to give 1-(6-chloro-5-cyanopyrazin-2-ylamino)cyclobutanecarboxamide (22 mg).

後処理

  1. customOrganic phase was separated
  2. washwashed with 1N HCl
  3. dry with materialwith 5% NaHCO3, dried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by HPLC

出典と根拠

ORDレコード
ord-9b932c5a0c204f47bdaa5045a8c95119
出典データセット
uspto-grants-2016_06
特許番号
US09359308B2

反応ノート

読み込み中…