Triethylamine → HCID 178512394, 화합물

HRID 77507

반응식

HRID 77507 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 197853Quinuclidine, 3-amino-, dihydrochlorideHCID 1404443183,5-Diamino-6-chloro-N-[(methylsulfanyl)methanimidoyl]pyrazine-2-carboxamide2회

생성물 1

HCID 178512394HCID 178512394, 화합물수율 15.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-51243bcc145f4f6d952cda21f136ef1f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841309B2

연결된 노트

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