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

Ammonium Chloride → HCID 86682466, 화합물

HRID 715891
노트
인쇄 미리보기

반응식

HRID 715891 반응식
[F:1][C:2]1([F:47])[CH2:7][CH2:6][CH:5]([C:8]2[C:17]3[CH:16]([OH:18])[CH2:15][C:14]([CH3:20])([CH3:19])[CH2:13][C:12]=3[N:11]=[C:10]([CH:21]3[CH2:26][CH2:25][N:24]([C:27]4[N:32]=[CH:31][C:30]([CH:33]=O)=[CH:29][N:28]=4)[CH2:23][CH2:22]3)[C:9]=2[CH:35]([F:46])[C:36]2[CH:41]=[CH:40][C:39]([C:42]([F:45])([F:44])[F:43])=[CH:38][CH:37]=2)[CH2:4][CH2:3]1.[CH3:48][NH2:49].CO.[BH4-].[Na+].[Cl-].[NH4+].C(=O)([O-])O.[Na+]>O1CCCC1.CO>[F:1][C:2]1([F:47])[CH2:3][CH2:4][CH:5]([C:8]2[C:17]3[CH:16]([OH:18])[CH2:15][C:14]([CH3:19])([CH3:20])[CH2:13][C:12]=3[N:11]=[C:10]([CH:21]3[CH2:26][CH2:25][N:24]([C:27]4[N:32]=[CH:31][C:30]([CH2:33][NH:49][CH3:48])=[CH:29][N:28]=4)[CH2:23][CH2:22]3)[C:9]=2[CH:35]([F:46])[C:36]2[CH:37]=[CH:38][C:39]([C:42]([F:45])([F:43])[F:44])=[CH:40][CH:41]=2)[CH2:6][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 25517Ammonium ChlorideHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydrideHCID 57454252Monomethylamine methanolHCID 86682450HCID 86682450, 화합물

생성물 1

HCID 86682466HCID 86682466, 화합물수율 76%

시약·촉매·용매

2
HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To 165 mg (0.250 mmol) of 4-(4,4-Difluorocyclohexyl)-3-{fluoro[4-(trifluoromethyl)phenyl]methyl}-2-[1-(5-formyl pyrimidin-2-yl)piperidin-4-yl]-7,7-dimethyl-5,6,7,8-tetrahydroquinolin-5-ol, which was prepared by a method similar to that of Example (36-1), 1.0 ml of methanol, 0.1 ml of tetrahydrofuran and 0.20 ml (about 2.5 mmol) of about 40% methylamine-methanol solution were added, and the reaction solution was stirred at room temperature for 12 hours. Then, 95 mg (2.5 mmol) of sodium borohydride was added thereto and the reaction solution was stirred at room temperature for 1 hour. After completion of the reaction, saturated ammonium chloride aqueous solution was poured into the reaction solution until the bubbling disappeared. Saturated sodium hydrogencarbonate aqueous solution was poured into the reaction solution to make the reaction solution basic and the reaction solution was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride aqueous solution and dried with anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The obtained residue was subjected to silica gel column chromatography [dichloromethane/methanol/28% ammonia water=100/0/0-90/9.5/0.5 (V/V/V)] and the fraction including the desired compound was concentrated under reduced pressure to provide 128 mg of the title compound as a colorless oil (yield: 76%).

후처리

  1. additionwere added
  2. stirringthe reaction solution was stirred at room temperature for 1 hour
  3. additionwas poured into the reaction solution until the bubbling
  4. extractionthe reaction solution was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated sodium chloride aqueous solution
  6. dry with materialdried with anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ea5fba7579c14e4a9323503a7e1cc190
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187450B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트