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

Potassium Hydroxide → (1, 1-dimethyl-2-(4-oxo-5-(2'-(N-triphenylmethyltetrazol-5-yl)biphenyl-4-ylmethyl)-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepin-3-ylcarbamoyl)ethyl)-carbamic acid tert-butyl ester

HRID 398787
노트
인쇄 미리보기

반응식

HRID 398787 반응식
[OH-].[K+].[C:3]([O:7][C:8](=[O:33])[NH:9][C:10]([CH3:32])([CH3:31])[CH2:11][C:12](=[O:30])[NH:13][CH:14]1[C:20](=[O:21])[NH:19][C:18]2[CH:22]=[CH:23][C:24]3[C:29]([C:17]=2[CH2:16][CH2:15]1)=[CH:28][CH:27]=[CH:26][CH:25]=3)([CH3:6])([CH3:5])[CH3:4].Br[CH2:35][C:36]1[CH:41]=[CH:40][C:39]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][C:43]=2[C:48]2[N:52]([C:53]([C:66]3[CH:71]=[CH:70][CH:69]=[CH:68][CH:67]=3)([C:60]3[CH:65]=[CH:64][CH:63]=[CH:62][CH:61]=3)[C:54]3[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=3)[N:51]=[N:50][N:49]=2)=[CH:38][CH:37]=1.[Cl-].[NH4+]>CS(C)=O.C(OCC)(=O)C.O>[C:3]([O:7][C:8](=[O:33])[NH:9][C:10]([CH3:32])([CH3:31])[CH2:11][C:12](=[O:30])[NH:13][CH:14]1[C:20](=[O:21])[N:19]([CH2:35][C:36]2[CH:37]=[CH:38][C:39]([C:42]3[CH:47]=[CH:46][CH:45]=[CH:44][C:43]=3[C:48]3[N:52]([C:53]([C:66]4[CH:71]=[CH:70][CH:69]=[CH:68][CH:67]=4)([C:60]4[CH:61]=[CH:62][CH:63]=[CH:64][CH:65]=4)[C:54]4[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=4)[N:51]=[N:50][N:49]=3)=[CH:40][CH:41]=2)[C:18]2[CH:22]=[CH:23][C:24]3[C:29]([C:17]=2[CH2:16][CH2:15]1)=[CH:28][CH:27]=[CH:26][CH:25]=3)([CH3:6])([CH3:4])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 14797Potassium HydroxideHCID 25517Ammonium ChlorideHCID 100534615-(4'-(Bromomethyl)(1,1'-biphenyl)-2-yl)-1-trityl-1H-tetraazoleHCID 53757316HCID 53757316, 화합물

생성물 1

HCID 54197216(1, 1-dimethyl-2-(4-oxo-5-(2'-(N-triphenylmethyltetrazol-5-yl)biphenyl-4-ylmethyl)-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepin-3-ylcarbamoyl)ethyl)-carbamic acid tert-butyl ester
수율 49.9%

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of dry powdered potassium hydroxide (0.23 g, 4.0 mmol) and (1,1-dimethyl-2-(4-oxo-2,3,4,5-tetrahydro-1H-naphtho[2,1-b]azepin-3-ylcarbamoyl)ethyl)carbamic acid tert-butyl ester (0.49 g, 1.0 mmol) in DMSO (15 ml) was stirred for 0.5 h under an atmosphere of nitrogen. 5-(4'-Bromomethyl-biphenyl-2-yl)-N-(triphenylmethyl)tetrazole (0.59 g, 1.1 mmol) was added and the mixture was stirred for 1 h. A 10% aqueous solution of ammoniumchloride (30 ml), water (100 ml) and ethyl acetate (60 ml) were added and the phases were separated. The organic layer was dried (MgSO4), and the solvent was evaporated in vacuo. Purification by columm chromatography on silica gel (100 g) using heptane and ethyl acetate (2:3) as eluent afforded 0.45 g of (1, 1-dimethyl-2-(4-oxo-5-(2'-(N -triphenylmethyltetrazol-5-yl)biphenyl-4-ylmethyl)-2,3,4,5-tetrahydro- 1H-naphtho[2,1-b]azepin-3-ylcarbamoyl)ethyl)- carbamic acid tert-butyl ester.

후처리

  1. customthe phases were separated
  2. dry with materialThe organic layer was dried (MgSO4)
  3. customthe solvent was evaporated in vacuo
  4. customPurification by columm chromatography on silica gel (100 g)

출처 및 근거

ORD 기록
ord-4869f446593941db911bb109f2058444
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05817654

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트