Methanol → HCID 178521002, 화합물

HRID 931293노트

반응식

HRID 931293 반응식
[NH2:1][C:2]1[C:7]([NH:8][C:9]([C:11]2([C:14]3[CH:19]=[N:18][CH:17]=[CH:16][N:15]=3)[CH2:13][CH2:12]2)=O)=[CH:6][CH:5]=[C:4]([N:20]2[CH2:25][CH2:24][CH2:23][C@@H:22]([C:26]([N:28]3[CH2:32][CH2:31][CH2:30][CH2:29]3)=[O:27])[CH2:21]2)[N:3]=1.CO.C[O-].[Na+]>C(O)C(C)C>[N:15]1[CH:16]=[CH:17][N:18]=[CH:19][C:14]=1[C:11]1([C:9]2[NH:1][C:2]3=[N:3][C:4]([N:20]4[CH2:25][CH2:24][CH2:23][C@@H:22]([C:26]([N:28]5[CH2:32][CH2:31][CH2:30][CH2:29]5)=[O:27])[CH2:21]4)=[CH:5][CH:6]=[C:7]3[N:8]=2)[CH2:13][CH2:12]1

참가 물질

5

반응물 3

HCID 887MethanolHCID 10942334Sodium MethoxideHCID 117966520HCID 117966520, 화합물

생성물 1

HCID 178521002HCID 178521002, 화합물수율 20.7%

시약·촉매·용매 1

HCID 6560Isobutanol용매

반응 조건

온도
100 °C

실험 절차

To a solution of (R)—N-(2-amino-6-(3-(pyrrolidine-1-carbonyl)piperidin-1-yl)pyridin-3-yl)-1-(pyrazin-2-yl)cyclopropanecarboxamide (0.1 g, 0.22 mmol) in anhydrous methanol (0.072 mL, 1.78 mmol) was added sodium methoxide (54 mg, 1.1 mmol) and isobutanol (3.5 mL). The reaction mixture was heated at 100° C. for 18 h. The solvent was removed under reduced pressure and the crude material was purified via preparative TLC to afford the title compound (19 mg). MS (ES+APCI) (M+H) 418.1; LCMS retention time 4.792 min (Method R1).

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe crude material was purified via preparative TLC

출처 및 근거

ORD 기록
ord-15fe885cdafb4c3b8b422ddcbe7ce2ad
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296745B2

반응 노트

불러오는 중…