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

Iodoethane → HCID 10220644, 화합물

HRID 1450173
노트
인쇄 미리보기

반응식

HRID 1450173 반응식
[H-].[Na+].[CH3:3][C:4]1[C:9]2[NH:10][C:11](=[O:19])[C:12]3[CH:18]=[CH:17][CH:16]=[N:15][C:13]=3[NH:14][C:8]=2[CH:7]=[CH:6][CH:5]=1.[CH2:20](I)[CH3:21]>CN(C=O)C>[CH2:20]([O:19][C:11]1[C:12]2[CH:18]=[CH:17][CH:16]=[N:15][C:13]=2[NH:14][C:8]2[CH:7]=[CH:6][CH:5]=[C:4]([CH3:3])[C:9]=2[N:10]=1)[CH3:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 4532707-Methyl-6,11-dihydro-5H-pyrido(2,3-b)(1,5)benzodiazepin-5-one

생성물 1

HCID 10220644HCID 10220644, 화합물수율 18.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

Sodium hydride (80% oil dispersion, 0.13 g, 5.5 mmol) was added at room temperature to a suspension of 6,11-dihydro-7-methyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one (1.12 g, 5.0 mmol) in DMF (20 mL) under argon. The reaction mixture was heated at 60° C. for 1 h and then was cooled in an ice-bath before the addition of ethyl iodide (0.86 g, 5.5 mmol). Stirring was continued at room temperature overnight, followed by warming to 60° C. for 1 h. The solution was concentrated in vacuo to near dryness, the residue was poured over ice-water, and the resulting solid was collected, washed with water, and dried. Purification by chromatography (elution with 1% MeOH/CH2Cl2) afforded 0.23 g (18%) of the title compound, which crystallized as yellow needles from petroleum ether (30°-60° C.): m.p. 135°-136° C.

후처리

  1. temperatureby warming to 60° C. for 1 h
  2. concentrationThe solution was concentrated in vacuo
  3. additionthe residue was poured over ice-water
  4. customthe resulting solid was collected
  5. washwashed with water
  6. customdried
  7. customPurification
  8. washby chromatography (elution with 1% MeOH/CH2Cl2)

출처 및 근거

ORD 기록
ord-0469e021ca2949c1be708f08ec1a7ca4
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05602113

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트