Triethylamine → HCID 178512394、化合物

HRID 77507

反応式

HRID 77507 の反応式
[NH2:1][C:2]1[C:3]([C:10]([NH:12][C:13](SC)=[NH:14])=[O:11])=[N:4][C:5]([Cl:9])=[C:6]([NH2:8])[N:7]=1.Cl.Cl.[NH2:19][CH:20]1[CH:25]2[CH2:26][CH2:27][N:22]([CH2:23][CH2:24]2)[CH2:21]1.C(N(CC)CC)C>O1CCCC1>[N:22]12[CH2:27][CH2:26][CH:25]([CH2:24][CH2:23]1)[CH:20]([NH:19][C:13]([NH:12][C:10]([C:3]1[C:2]([NH2:1])=[N:7][C:6]([NH2:8])=[C:5]([Cl:9])[N:4]=1)=[O:11])=[NH:14])[CH2:21]2

参加物

5

反応物 3

HCID 8471TriethylamineHCID 197853Quinuclidine, 3-amino-, dihydrochlorideHCID 1404443183,5-Diamino-6-chloro-N-[(methylsulfanyl)methanimidoyl]pyrazine-2-carboxamide2 回

生成物 1

HCID 178512394HCID 178512394、化合物収率 15.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

3,5-Diamino-6-chloro-N-[(methylsulfanyl)methanimidoyl]pyrazine-2-carboxamide (Intermediate 3, 250 mg, 0.88 mmol) is dissolved in tetrahydrofuran (20 mL) and to the solution 3-amino-quinuclidine dihydrochloride (211 mg, 1.06 mmol) and triethylamine (0.61 mL, 4.41 mmol) are added. The mixture is heated at 80° C. for 24 hours. The solid is removed by filtration and the is filtrate evaporated and purified by preparative HPLC (5 mM ammonium formate in H2O: CH3CN gradient) obtaining the title compound (45 mg).

後処理

  1. additionare added
  2. customThe solid is removed by filtration
  3. customthe is filtrate evaporated
  4. custompurified by preparative HPLC (5 mM ammonium formate in H2O: CH3CN gradient)

出典と根拠

ORDレコード
ord-51243bcc145f4f6d952cda21f136ef1f
出典データセット
uspto-grants-2014_09
特許番号
US08841309B2

関連ノート

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