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

Hydroxyamine hydrochloride → HCID 11197008, 화합물

HRID 509189
노트
인쇄 미리보기

반응식

HRID 509189 반응식
[CH:1]([N:14]1C(C2C=CC(OC)=CC=2)[O:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.NO>CO>[CH:1]([NH:14][OH:15])([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 13635628HCID 13635628, 화합물

생성물 1

HCID 11197008HCID 11197008, 화합물수율 20.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 2-benzhydryl-3-(4-methoxyphenyl)-1,2-oxaziridine 40 (3.52 g, 11.1 mmol) in methanol (100 mL) was added hydroxylamine-HCl (2.31 g, 33.3 mmol) and stirred at room temperature. for 16 h. The reaction mixture was concentrated under vacuum and diluted with aqueous NaOH solution (to pH=13), followed by extraction with ethyl acetate. The combined organic layers were dried over anhydrous Na2SO4, filtered, and concentrated. The crude material was concentrated and purified by silica gel column chromatography with gradient of ethyl acetate (10-50%) in hexane to afford compound 41 as a light yellow solid (450 mg, 20%). LRMS (ESI): (calc.) 199.3 (found) 167.2 (M-NHOH)+.

후처리

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. additiondiluted with aqueous NaOH solution (to pH=13)
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. concentrationThe crude material was concentrated
  8. custompurified by silica gel column chromatography with gradient of ethyl acetate (10-50%) in hexane

출처 및 근거

ORD 기록
ord-3745e57776ff473899db7ca4c4c6fd83
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096565B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트