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

Cesium carbonate → (3-Pyrrolidin-1-ylphenyl)methylamine

HRID 2041161
노트
인쇄 미리보기

반응식

HRID 2041161 반응식
C(OC(=O)[NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11](Br)[CH:10]=1)(C)(C)C.[NH:17]1[CH2:21][CH2:20][CH2:19][CH2:18]1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[N:17]1([C:11]2[CH:10]=[C:9]([CH:14]=[CH:13][CH:12]=2)[CH2:8][NH2:7])[CH2:21][CH2:20][CH2:19][CH2:18]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 31268PyrrolidineHCID 634876Binap, (A+-)-HCID 11033439tert-Butyl 3-bromobenzylcarbamate

생성물 1

HCID 7162061(3-Pyrrolidin-1-ylphenyl)methylamine수율 85%

시약·촉매·용매 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매

반응 조건

온도
90 °C

실험 절차

Slurry a mixture of (3-bromobenzyl)-carbamic acid tert-butyl ester (600 mg, 2.1 mmol, U.S. Pat. Appl. Publ. US 2003134885), pyrrolidine (450 mL, 5.2 mmol), tris(dibenzylideneacetone)dipalladium(0) (200 mg, 0.21 mmol), BINAP (400 mg, 0.63 mmol) and cesium carbonate (960 mg, 2.94 mmol) in anhydrous toluene (10 mL). Degas under vacuum, fill the system with nitrogen and heat in a sealed flask at 90° C. for 18 h. Cool to room temperature, dilute with diethyl ether, filter, and concentrate in vacuo. Dissolve the resulting residue in DCM (10 mL) and add trifluoroacetic acid (5 mL). Stir at ambient temperature for 1 h and concentrate in vacuo. Purify by chromatography on silica gel eluting sequentially with hexane/EtOAc (1:1), EtOAc and 2M ammonia in methanol. Purify again by SCX chromatography to give the title compound as a brown oil (300 mg, 85% overall). MS (ES+) m/z: 178 (M+H)+.

후처리

  1. customDegas under vacuum
  2. temperatureCool to room temperature
  3. additiondilute with diethyl ether
  4. filtrationfilter
  5. concentrationconcentrate in vacuo
  6. dissolutionDissolve the resulting residue in DCM (10 mL)
  7. additionadd trifluoroacetic acid (5 mL)
  8. concentrationconcentrate in vacuo
  9. customPurify by chromatography on silica gel eluting sequentially with hexane/EtOAc (1:1), EtOAc and 2M ammonia in methanol
  10. customPurify again by SCX chromatography

출처 및 근거

ORD 기록
ord-c01dd05d07184fe68ce9b050a246afe3
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08580780B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트