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

Formaldehyde → 2-Methyl-11-[4-methyl-(S)-3-phenethyl-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine

HRID 1350516
노트
인쇄 미리보기

반응식

HRID 1350516 반응식
[CH3:1][C:2]1[CH:30]=[CH:29][C:5]2[NH:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[N:9]=[C:10]([N:11]3[CH2:16][CH2:15][NH:14][C@@H:13]([CH2:17][CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH2:12]3)[C:4]=2[CH:3]=1.C=O.[C:33](O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCCl>[CH3:1][C:2]1[CH:30]=[CH:29][C:5]2[NH:6][C:7]3[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=3[N:9]=[C:10]([N:11]3[CH2:16][CH2:15][N:14]([CH3:33])[C@@H:13]([CH2:17][CH2:18][C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH2:12]3)[C:4]=2[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 5049666Sodium triacetoxyborohydrideHCID 588606152-Methyl-11-[(S)-3-phenethyl-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine

생성물 1

HCID 210934992-Methyl-11-[4-methyl-(S)-3-phenethyl-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine수율 90%

시약·촉매·용매 1

HCID 111,2-Dichloroethane
용매

실험 절차

Combine 2-methyl-11-[(S)-3-phenethyl-piperazin-1-yl]-5H-dibenzo[b,e][1,4]diazepine (300.0 mg, 0.76 mmol), formaldehyde (67.5 μL, 0.83 mmol, 37% in water), and 1,2-dichloroethane (25.0 ml). Stir the mixture at ambient temperature for 5 minutes and then add sodium triacetoxyborohydride (240.5 mg, 1.13 mmol). After stirring for 30 minutes at ambient temperature, quench the reaction with saturated sodium bicarbonate. Remove the organic portion and wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Purify the residue on silica gel using dichloromethane/methanol (90:10) to give 279.7 mg (90%) of the title compound as a yellow foam: mp 65°, dec; mass spectrum (ion spray): m/z=411.2 (M+1).

후처리

  1. stirringAfter stirring for 30 minutes at ambient temperature
  2. customquench
  3. customthe reaction with saturated sodium bicarbonate
  4. customRemove the organic portion
  5. washwash (brine)
  6. dry with materialdry (sodium sulfate)
  7. customPurify the residue on silica gel

출처 및 근거

ORD 기록
ord-66f80f38c90347a19fb34eb5e612dd02
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214673B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트