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

Sodium Sulfate → HCID 178487982, 화합물

HRID 657129
노트
인쇄 미리보기

반응식

HRID 657129 반응식
[NH2:1][CH2:2][C@@H:3]1[CH2:8][CH2:7][CH2:6][N:5]([CH2:9][CH2:10][N:11]2[C:16](=[O:17])[CH:15]=[N:14][C:13]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[N:21][C:12]2=3)[CH2:4]1.[O:24]=[C:25]1[NH:36][C:29]2[N:30]=[C:31]([CH:34]=O)[N:32]=[CH:33][C:28]=2[CH2:27][CH2:26]1.[O-]S([O-])(=O)=O.[Na+].[Na+].[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].CO.C(Cl)[Cl:61]>>[ClH:61].[ClH:61].[CH3:23][O:22][C:20]1[CH:19]=[CH:18][C:13]2[N:14]=[CH:15][C:16](=[O:17])[N:11]([CH2:10][CH2:9][N:5]3[CH2:6][CH2:7][CH2:8][C@@H:3]([CH2:2][NH:1][CH2:34][C:31]4[NH:30][C:29]5=[N:36][C:25](=[O:24])[CH2:26][CH2:27][C:28]5=[CH:33][N:32]=4)[CH2:4]3)[C:12]=2[N:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 24436Sodium SulfateHCID 5049666Sodium triacetoxyborohydrideHCID 21226129Dichloromethane methanolHCID 594374057-Oxo-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine-2-carbaldehyde2회HCID 689911274-{2-[(3S)-3-(Aminomethyl)-1-piperidinyl]ethyl}-6-(methyloxy)pyrido[2,3-b]pyrazin-3(4H)-one

생성물 1

HCID 178487982
HCID 178487982, 화합물

실험 절차

To a solution of 4-{2-[(3S)-3-(aminomethyl)-1-piperidinyl]ethyl}-6-(methyloxy)pyrido[2,3-b]pyrazin-3(4H)-one (0.072 g, 0.23 mmol) in 1:1 MeOH/DCM (20 mL), was added 7-oxo-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine-2-carbaldehyde (for a preparation see Example 125(c)) (0.04 g, 0.23 mmol), and excess Na2SO4. The solution was stirred at ambient temperature for 16 h followed by the addition of NaBH(OAc)3 (1.68 g, 7.92 mmol). The resulting solution was stirred for an additional 2 hours. Analysis by LCMS showed only 50% product, therefore an additional portion of 7-oxo-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine-2-carbaldehyde (0.04 g, 0.23 mmol) was added and the reaction was stirred for an additional 16 h. The solution was then concentrated onto silica gel under vacuum and the crude residue purified by column chromatography (silica gel) using a DCM/DCM-MeOH—NH4OH (90:10:1) gradient to yield the free base of the desired product as a yellow oily film (0.034 g, 32%). LCMS: m/z 479.2 (MH+). 1H NMR (400 MHz, CDCl3) δ 1.57-1.69 (m, 2H) 1.73-1.82 (m, 1H) 1.95 (d, J=8.59 Hz, 21H) 2.18 (td, J=10.99, 3.03 Hz, 1H) 2.51-2.63 (m, 21H) 2.67-2.75 (m, 4H) 2.81-2.92 (m, 1H) 2.92-3.01 (m, 2H) 3.21-3.32 (m, 1H) 3.88-4.00 (m, 2H) 4.00-4.05 (m, 3H) 4.57-4.68 (m, 2H) 6.73 (d, J=8.59 Hz, 1H) 8.00-8.04 (m, 1H) 8.23 (s, 1H) 8.36 (s, 1H).

후처리

  1. stirringThe resulting solution was stirred for an additional 2 hours
  2. stirringthe reaction was stirred for an additional 16 h
  3. concentrationThe solution was then concentrated onto silica gel under vacuum
  4. customthe crude residue purified by column chromatography (silica gel)

출처 및 근거

ORD 기록
ord-9352693a628e4a71b8bee9912095b3a8
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08071592B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트