홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethanol → HCID 178419985, 화합물

HRID 931262
노트
인쇄 미리보기

반응식

HRID 931262 반응식
[N:1]1[N:2]=[C:3]([CH:9]2[CH2:14][CH2:13][CH2:12][N:11]([C:15]3[N:20]=[C:19]([NH2:21])[C:18]([N+:22]([O-])=O)=[CH:17][CH:16]=3)[CH2:10]2)[N:4]2[CH2:8][CH2:7][CH2:6][C:5]=12.[CH:25]1([C:28]2[CH:33]=[CH:32][CH:31]=[C:30]([CH:34]=O)[N:29]=2)[CH2:27][CH2:26]1.S(S([O-])=O)([O-])=O.[Na+].[Na+].C(O)C>O>[CH:25]1([C:28]2[N:29]=[C:30]([C:34]3[NH:21][C:19]4=[N:20][C:15]([N:11]5[CH2:12][CH2:13][CH2:14][CH:9]([C:3]6[N:4]7[CH2:8][CH2:7][CH2:6][C:5]7=[N:1][N:2]=6)[CH2:10]5)=[CH:16][CH:17]=[C:18]4[N:22]=3)[CH:31]=[CH:32][CH:33]=2)[CH2:27][CH2:26]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 702EthanolHCID 24489Sodium DithioniteHCID 193617216-CyclopropylpicolinaldehydeHCID 898542026-(3-(6,7-dihydro-5H-pyrrolo[2,1-c][1,2,4]triazol-3-yl)piperidin-1-yl)-3-nitropyridin-2-amine2회

생성물 1

HCID 178419985HCID 178419985, 화합물수율 21%

시약·촉매·용매 1

HCID 962
Water
용매

반응 조건

온도
110 °C

실험 절차

A mixture of 6-(3-(6,7-dihydro-5H-pyrrolo[2,1-c][1,2,4]triazol-3-yl)piperidin-1-yl)-3-nitropyridin-2-amine (Intermediate 45) (300 mg, 0.91 mmol), 2-cyclopropylpyridine-6-aldehyde (187.5 mg, 1.27 mmol), sodium dithionite (602.6 mg, 4.46 mmol), ethanol (15 mL) and water (2.4 mL) in a sealed tube was heated to 110° C. for 16 h. The mixture was concentrated under reduced pressure and the residue was partitioned between ethyl acetate and water. The organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was and purified via preparative TLC to afford the title compound (80 mg, 21%) as a racemic mixture. MS (ES+) (M+H) 427.3; LCMS retention time 2.687 min (Method J). 1H NMR (400 MHz, CDCl3) δ 1.02-1.15 (m, 4H), 1.73-1.82 (m, 1H), 1.89-2.13 (m, 3H), 2.21 (d, 1H), 2.74-2.85 (m, 2H), 2.94-3.01 (m, 2H), 3.02-3.12 (m, 2H), 3.21-3.32 (m, 1H), 3.91-4.10 (m, 2H), 4.33 (d, 1H), 4.65 (d, 1H), 6.75 (d, 1H), 7.20 (d, 1H), 7.66 (t, 2H), 7.88 (d, 1H), 8.05 (d, 1H), 10.20 (br s, 1H).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and water
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. custompurified via preparative TLC

출처 및 근거

ORD 기록
ord-5da4bbb99d2a4e2abc4a98809079b05e
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트