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

Piperidine → HCID 10108875, 화합물

HRID 1635916
노트
인쇄 미리보기

반응식

HRID 1635916 반응식
[C:1]1([C:7]2[N:11]3[CH:12]=[C:13]([C:20]([OH:22])=O)[C:14]4[C:19]([C:10]3=[CH:9][N:8]=2)=[CH:18][CH:17]=[CH:16][CH:15]=4)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.F[P-](F)(F)(F)(F)F.[N:30]1(O[P+](N(C)C)(N(C)C)N(C)C)[C:34]2C=[CH:36][CH:37]=[CH:38][C:33]=2N=N1.N1CCCCC1.C([O-])(O)=O.[Na+]>CN(C=O)C>[C:1]1([C:7]2[N:11]3[CH:12]=[C:13]([C:20]([N:30]4[CH2:36][CH2:37][CH2:38][CH2:33][CH2:34]4)=[O:22])[C:14]4[C:19]([C:10]3=[CH:9][N:8]=2)=[CH:18][CH:17]=[CH:16][CH:15]=4)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8082PiperidineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 516892Sodium BicarbonateHCID 22136183HCID 22136183, 화합물

생성물 1

HCID 10108875HCID 10108875, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

A mixture of the product from part 9 (95 mg), BOP (220 mg), piperidine (56 mg) and TEA (67 mg) in 2 ml of DMF is stirred at room temperature for 18 hours. The mixture is added to aqueous NaHCO3 solution and extracted with EtOAc. The organic layer is washed with brine and water, dried (Na2SO4), filtered and concentrated to afford a foam. Purification on a silica gel column, eluting with 5% methanol in methylene chloride, gives the title compound. 1H NMR (CDCl3) δ 1.38-1.50 and 1.60-1.80 (6H, m), 3.18-3.36 (2H, m), 3.65-3.95 (2H, m), 7.40-7.60 (6H, m), 7.75 (2H, d), 7.95 (1H, s), 8.05 (1H, s), 8.10 (1H, d). The hydrochloride salt was prepared by treating the free base in EtOAc with a solution of hydrogen chloride in ether and collecting by filtration.

후처리

  1. extractionextracted with EtOAc
  2. washThe organic layer is washed with brine and water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto afford a foam
  7. customPurification on a silica gel column
  8. washeluting with 5% methanol in methylene chloride

출처 및 근거

ORD 기록
ord-919e7cc1469b462195e35456f3277ac1
출처 데이터셋
uspto-grants-2003_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06511987B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트