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

Diethylamine → N,N-diethyl-5-(1-methyl-1,2,3,4-tetrazol-5-yl)valeramide

HRID 978033
노트
인쇄 미리보기

반응식

HRID 978033 반응식
[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=O)=[N:5][N:4]=[N:3]1.[CH2:14]([N:16](CC)[CH2:17][CH3:18])[CH3:15].ClC(OCC(C)C)=O.C(NCC)C>CN(C)C=O>[CH2:14]([N:16]([CH2:17][CH3:18])[C:11](=[O:13])[CH2:10][CH2:9][CH2:8][CH2:7][C:6]1[N:2]([CH3:1])[N:3]=[N:4][N:5]=1)[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8021DiethylamineHCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 132034015-(1-Methyl-1,2,3,4-tetrazol-5-yl)valeric acid

생성물 1

HCID 13142190N,N-diethyl-5-(1-methyl-1,2,3,4-tetrazol-5-yl)valeramide수율 29.9%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

5-(1-Methyl-1,2,3,4-tetrazol-5-yl)valeric acid (1.8 g) is dissolved in dimethylformamide (50 ml), and thereto is added triethylamine (1.1 g). To the mixture is added dropwise with stirring isobutyl chloroformate (1.5 g) under ice-cooling, and the mixture is stirred at room temperature for 30 minutes. To the mixture is added dropwise with stirring diethylamine (0.9 g) at rood temperature, and the mixture is stirred for 2 hours. Dimethylformamide is distilled off under reduced pressure, and the residue is purified by column chromatography (Wakogel C-200). After eluting with benzene-chloroform (1:1), the eluate is distilled under reduced pressure to give N,N-diethyl-5-(1-methyl-1,2,3,4-tetrazol-5-yl)-valeramide (0.7 g), colorless liquid, b.p. 190°-200° C. (bath temperature)/0.07 mmHg, nD25 =1.4907.

후처리

  1. temperaturecooling
  2. stirringthe mixture is stirred for 2 hours
  3. distillationDimethylformamide is distilled off under reduced pressure
  4. customthe residue is purified by column chromatography (Wakogel C-200)
  5. washAfter eluting with benzene-chloroform (1:1)
  6. distillationthe eluate is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-54a12651ee4c4d3f80e6dc3a2001c718
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04663323

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트