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

Sodium hydride → HCID 20393023, 화합물

HRID 1862983
노트
인쇄 미리보기

반응식

HRID 1862983 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH3:21])[C:5]2[C:11](=[O:12])[N:10]([CH3:13])[C:9]3[CH:14]=[C:15]([CH3:19])[C:16]([CH3:18])=[CH:17][C:8]=3[NH:7][C:6]=2[N:20]=1.[H-].[Na+].[CH2:24]([N:26]([CH2:31][CH3:32])[CH2:27][CH2:28][CH2:29]Cl)[CH3:25]>CN(C)C=O>[CH2:24]([N:26]([CH2:31][CH3:32])[CH2:27][CH2:28][CH2:29][N:7]1[C:8]2[CH:17]=[C:16]([CH3:18])[C:15]([CH3:19])=[CH:14][C:9]=2[N:10]([CH3:13])[C:11](=[O:12])[C:5]2[C:4]([CH3:21])=[CH:3][C:2]([CH3:1])=[N:20][C:6]1=2)[CH3:25]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 669183-Chloropropyl(diethyl)amineHCID 23372624HCID 23372624, 화합물

생성물 1

HCID 20393023HCID 20393023, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
50 °C

실험 절차

A mixture consisting of 1.8 mg of 6,11-dihydro-2,4,6,8,9-pentamethyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, 30 ml of dimethyl formamide and 0.34 gm of 50% sodium hydride in mineral oil was stirred in a nitrogen atmosphere at 50° C. for 30 minutes. Then, a solution of 1.5 gm of 3-diethylaminopropyl chloride in 15 ml of dimethyl formamide was added dropwise at room temperature, and the mixture was heated on an oil bath at 120° C. for 2 hours and then evaporated in vacuo. The residue was admixed with dilute ammonia, and the mixture was repeatedly extracted with ether. The combined ether extracts were dried with sodium sulfate, the ether was distilled off, and the residue was recrystallized from petroleum ether (m.p. 100°-140° C.), yielding 53% of theory of the compound named in the heading, which had a melting point of 104°-106° C.

후처리

  1. temperaturethe mixture was heated on an oil bath at 120° C. for 2 hours
  2. customevaporated in vacuo
  3. extractionthe mixture was repeatedly extracted with ether
  4. dry with materialThe combined ether extracts were dried with sodium sulfate
  5. distillationthe ether was distilled off
  6. customthe residue was recrystallized from petroleum ether (m.p. 100°-140° C.)
  7. customyielding 53% of theory of the compound

출처 및 근거

ORD 기록
ord-946780e0377a43a4af75cee4ce5ad33b
출처 데이터셋
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04167570

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트