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

N'-(4-benzyloxy-3-cyano-pyridin-2-yl)-2-cyclopropylacetohydrazide → 7-Chloro-3-(cyclopropylmethyl)[1,2,4]triazolo[4,3-a]pyridine-8-carbonitrile

HRID 587626
노트
인쇄 미리보기

반응식

HRID 587626 반응식
[C:1]([C:3]1[C:4]([NH:17][NH:18][C:19](=O)[CH2:20][CH:21]2[CH2:23][CH2:22]2)=[N:5][CH:6]=[CH:7][C:8]=1OCC1C=CC=CC=1)#[N:2].O(Cl)[Cl:26].[P+5]>ClCCCl.C(Cl)Cl>[Cl:26][C:8]1[CH:7]=[CH:6][N:5]2[C:19]([CH2:20][CH:21]3[CH2:23][CH2:22]3)=[N:18][N:17]=[C:4]2[C:3]=1[C:1]#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 66784643N'-(4-benzyloxy-3-cyano-pyridin-2-yl)-2-cyclopropylacetohydrazideHCID 178479711HCID 178479711, 화합물

생성물 1

HCID 574595937-Chloro-3-(cyclopropylmethyl)[1,2,4]triazolo[4,3-a]pyridine-8-carbonitrile수율 64.3%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 6344Dichloromethane용매

실험 절차

A solution of D4 (1.4 g, 4.343 mmol) and phosphorous (V) oxychloride (0.810 ml, 8.686 mmol) in DCE (15 ml) was heated at 150° C. under microwave irradiation for 5 min. After cooling, the mixture was diluted with DCM and washed with NaHCO3 (aqueous sat. solution). The organic layer was separated, dried (Na2SO4) and concentrated in vacuo. The crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 2% as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate compound D5 (0.650 g, 64%).

후처리

  1. temperatureAfter cooling
  2. washwashed with NaHCO3 (aqueous sat. solution)
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by column chromatography (silica gel; DCM/7M solution of NH3 in MeOH up to 2% as eluent)
  7. customThe desired fractions were collected
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b835ef62fb544a199e93aa270eb2ce9d
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09226930B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트