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

Acetone → N-[3-({N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]amino}methyl)pyridin-2-ylmethyl]formamide

HRID 68973
노트
인쇄 미리보기

반응식

HRID 68973 반응식
[CH2:1]([N:3]1[C:9](=[O:10])[C:8]([CH3:12])([CH3:11])[C:7](=[O:13])[N:6]([CH3:14])[C:5]2[CH:15]=[C:16]([CH2:19][N:20]([CH2:34][C:35]3[C:36]([C:41]#[N:42])=[N:37][CH:38]=[CH:39][CH:40]=3)[CH2:21][CH2:22][N:23]3[CH:28]=[CH:27][C:26]4[O:29][C:30]([CH3:32])=[CH:31][C:25]=4[C:24]3=[O:33])[CH:17]=[CH:18][C:4]1=2)[CH3:2].C[C:44](C)=[O:45]>[Ni].C(O)=O>[CH2:1]([N:3]1[C:9](=[O:10])[C:8]([CH3:12])([CH3:11])[C:7](=[O:13])[N:6]([CH3:14])[C:5]2[CH:15]=[C:16]([CH2:19][N:20]([CH2:34][C:35]3[C:36]([CH2:41][NH:42][CH:44]=[O:45])=[N:37][CH:38]=[CH:39][CH:40]=3)[CH2:21][CH2:22][N:23]3[CH:28]=[CH:27][C:26]4[O:29][C:30]([CH3:32])=[CH:31][C:25]=4[C:24]3=[O:33])[CH:17]=[CH:18][C:4]1=2)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 180AcetoneHCID 706571733-({N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]amino}methyl)pyridine-2-carbonitrile

생성물 1

HCID 86670481N-[3-({N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]amino}methyl)pyridin-2-ylmethyl]formamide

시약·촉매·용매 2

HCID 935
Nickel
촉매
HCID 284Formic Acid용매

반응 조건

온도
60 °C

실험 절차

3-({N-(1-Ethyl-3,3,5-trimethyl-2,4-dioxo-2,3,4,5-tetrahydro-1H-benzo[b][1,4]diazepin-7-ylmethyl)-N-[2-(2-methyl-4-oxo-4H-furo[3,2-c]pyridin-5-yl)ethyl]amino}methyl)pyridine-2-carbonitrile (0.40 g) and Raney nickel (1.2 g) were suspended in formic acid (8 ml), and the mixture was stirred at 60° C. for 3 hours. The reaction mixture was filtered to remove insoluble matter, and the filtrate was condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:methanol=75:25→80:20). The purified product was condensed under reduced pressure. Acetone and ether were added to the residue. The precipitated insoluble matter was separated, washed with ether, and dried to give the title compound (33 mg) as a pale brown white amorphous.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customto remove insoluble matter
  3. customcondensed under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:methanol=75:25→80:20)
  5. customcondensed under reduced pressure
  6. customThe precipitated insoluble matter was separated
  7. washwashed with ether
  8. customdried

출처 및 근거

ORD 기록
ord-5bff13f594c7478eafb56771d2153e9c
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822453B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트