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

Ammonia → 10-bromo-3-(cyclopropanecarboxamidomethyl)-9-fluoro-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide

HRID 575323
노트
인쇄 미리보기

반응식

HRID 575323 반응식
[Br:1][C:2]1[C:3]([F:22])=[CH:4][C:5]2[CH:11]3[CH2:12][CH:9]([CH2:10]3)[N:8]3[C:13](C=O)=[C:14]([C:16]([NH2:18])=[O:17])[N:15]=[C:7]3[C:6]=2[CH:21]=1.[C:23]([O-:26])(=O)[CH3:24].[NH4+].[C:28]([BH3-])#[N:29].[Na+].N.[CH2:33](O)[CH3:34]>>[Br:1][C:2]1[C:3]([F:22])=[CH:4][C:5]2[CH:11]3[CH2:12][CH:9]([CH2:10]3)[N:8]3[C:13]([CH2:28][NH:29][C:23]([CH:24]4[CH2:34][CH2:33]4)=[O:26])=[C:14]([C:16]([NH2:18])=[O:17])[N:15]=[C:7]3[C:6]=2[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 222AmmoniaHCID 702EthanolHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 8669316110-bromo-9-fluoro-3-formyl-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide

생성물 1

HCID 86693359
10-bromo-3-(cyclopropanecarboxamidomethyl)-9-fluoro-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide

실험 절차

10-bromo-9-fluoro-3-formyl-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide (50 mg) was added into a saturated solution of ammonium acetate in Ethanol (2.7 mL) at which point sodium cyanoborohydride (3 eq) and 30% aqueous ammonia solution (1 mL) were added. The mixture was stirred at reflux for 1 hr, until reaction was deemed complete by LC-MS. The reaction was cooled to room temperature, concentrated to dryness and suspended in Methanol. The slurry was loaded onto a biotage scx-2 cartridge, rinsed with Methanol and crude 3-(aminomethyl)-10-bromo-9-fluoro-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide was then eluted with a 4N ammonia in methanol solution and concentrated to an orange oil. The crude intermediate was reacted with cyclopropane carboxylic acid similarly to as described in Example 2 to afford crude 10-bromo-3-(cyclopropanecarboxamidomethyl)-9-fluoro-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide which was directly reacted with 2-Methyl-3-butyne-ol via General Procedure E to afford 12 mg (33%) of 3-[(cyclopropanecarbonylamino)methyl]-9-fluoro-10-(3-hydroxy-3-methyl-but-1-ynyl)-5,6,7,12-tetrahydro-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide.

후처리

  1. additionwere added
  2. temperatureat reflux for 1 hr, until reaction
  3. concentrationconcentrated to dryness
  4. washrinsed with Methanol and crude 3-(aminomethyl)-10-bromo-9-fluoro-6,7-dihydro-5H-5,7-methanobenzo[c]imidazo[1,2-a]azepine-2-carboxamide
  5. washwas then eluted with a 4N ammonia in methanol solution
  6. concentrationconcentrated to an orange oil
  7. customThe crude intermediate was reacted with cyclopropane carboxylic acid similarly

출처 및 근거

ORD 기록
ord-a93c110df05c426ca7508e619c189e61
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09034866B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트