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

Triphenylphosphine → 3-(1-Amino-isoquinolin-6-yloxy)piperidin-1--carboxylic acid tert-butyl ester

HRID 1435963
노트
인쇄 미리보기

반응식

HRID 1435963 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][C@@H:10]([OH:14])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH2:34][C:35]1[C:44]2[C:39](=[CH:40][C:41](O)=[CH:42][CH:43]=2)[CH:38]=[CH:37][N:36]=1.CCOC(/N=N/C(OCC)=O)=O.[OH-].[Na+]>C1COCC1.CN(C=O)C.O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([O:14][C:41]2[CH:40]=[C:39]3[C:44](=[CH:43][CH:42]=2)[C:35]([NH2:34])=[N:36][CH:37]=[CH:38]3)[CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 1514398(R)-1-Boc-3-hydroxypiperidineHCID 5462977Diethyl azodicarboxylateHCID 1357539911-Aminoisoquinolin-6-ol

생성물 1

HCID 775634643-(1-Amino-isoquinolin-6-yloxy)piperidin-1--carboxylic acid tert-butyl ester
수율 20.2%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (R)-3-hydroxypiperidine-1-carboxylic acid tert-butyl ester (209 mg, 1.04 mmol), triphenylphosphine (327 mg, 1.249 mmol), 1-amino-isoquinolin-6-ol (200 mg, 1.249 mmol) in THF (4 ml) and DMF (394 μL) at 0° C., under argon, was added dropwise diethylazodicarboxylate (197 mL) over 5 min. The mixture was then warmed to ambient temperature and stirred for 48 h. Water was then added and the mixture basified with dilute NaOH. The mixture was extracted with ethyl acetate (X3), dried (sodium sulphate) filtered and evaporated under reduced pressure to give a residue. Flash chromatography of the residue on silica (eluent: 2-10% methanol in dichloromethane with 1% aqueous ammonia) gave (S) 3-(1-amino-isoquinolin-6-yloxy)piperidin-1--carboxylic acid tert-butyl ester (72 mg), El-MS: m/z=344.1 [M+H]+.

후처리

  1. extractionThe mixture was extracted with ethyl acetate (X3)
  2. dry with materialdried (sodium sulphate)
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customto give a residue

출처 및 근거

ORD 기록
ord-09d2470d721847ecba85d1d9cbd6ed5f
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618985B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트