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

Acetic Acid → Benzyl 1-methylspiro[indoline-3,4'-piperidine]-1'-carboxylate

HRID 390382
노트
인쇄 미리보기

반응식

HRID 390382 반응식
[N:1]1([C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:16])[CH2:6][CH2:5][C:4]2([C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[NH:8][CH2:7]2)[CH2:3][CH2:2]1.C=O.[C:27](O)(=O)C.C([BH3-])#N.[Na+].C([O-])(O)=O.[Na+]>CO>[CH3:27][N:8]1[C:9]2[C:14](=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:4]2([CH2:3][CH2:2][N:1]([C:15]([O:17][CH2:18][C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)=[O:16])[CH2:6][CH2:5]2)[CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 712FormaldehydeHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 10914256Benzyl 1,2-dihydrospiro[indole-3,4'-piperidine]-1'-carboxylate

생성물 1

HCID 18335092Benzyl 1-methylspiro[indoline-3,4'-piperidine]-1'-carboxylate수율 75.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a 0° C. solution of benzyl spiro[indoline-3,4′-piperidine]-1′-carboxylate (1.15 g, 3.56 mmol), formaldehyde (37% aqueous solution, 1.44 mL, 17.83 mmol) and acetic acid (1.02 mL, 17.83 mmol) in methanol (25 mL) is added sodium cyanoborohydride (0.67 g, 10.68 mmol). The reaction mixture is allowed to warm to room temperature overnight. The pH of the mixture is adjusted to approximately 8 with 10% NaHCO3 solution and extracted with EtOAc (3×50 mL). The combined extracts are washed with water (50 mL) and brine (50 mL), dried, filtered, and evaporated to dryness. The crude material is purified by silica gel chromatography, eluting with hexane:ethyl acetate (85:15) to give the title compound as an off-white solid (0.9 g, 75%). ESI/MS m/z 337.2 (M+H)+.

후처리

  1. extractionextracted with EtOAc (3×50 mL)
  2. washThe combined extracts are washed with water (50 mL) and brine (50 mL)
  3. customdried
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe crude material is purified by silica gel chromatography
  7. washeluting with hexane:ethyl acetate (85:15)

출처 및 근거

ORD 기록
ord-987ca30390754174bccf5de80f935aa9
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383642B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트