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

Triethylamine → trans-2-(2-Cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester

HRID 731289
노트
인쇄 미리보기

반응식

HRID 731289 반응식
Cl.[NH2:2][C@H:3]1[CH2:7][CH2:6][CH2:5][C@H:4]1[C:8]([O:10][CH2:11][CH3:12])=[O:9].C(N(CC)CC)C.[CH:20]1([CH2:23][CH:24]=O)[CH2:22][CH2:21]1.C([BH3-])#N.[Na+]>C(O)C>[CH2:11]([O:10][C:8]([C@@H:4]1[CH2:5][CH2:6][CH2:7][C@@H:3]1[NH:2][CH2:24][CH2:23][CH:20]1[CH2:22][CH2:21]1)=[O:9])[CH3:12].[CH2:11]([O:10][C:8]([C@@H:4]1[CH2:5][CH2:6][CH2:7][C@H:3]1[NH:2][CH2:24][CH2:23][CH:20]1[CH2:22][CH2:21]1)=[O:9])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 2725067rac-ethyl (1R,2S)-2-aminocyclopentane-1-carboxylate hydrochlorideHCID 5003444Sodium cyanoborohydrideHCID 103078492-Cyclopropylacetaldehyde

생성물 2

HCID 69061399trans-2-(2-Cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester수율 90.5%
HCID 69063495
cis-2-(2-Cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of cis-ethyl 2-amino-1-cyclopentanecarboxylate hydrochloride (250.0 mg, 1.28 mmol) in ethanol (5 mL) was added triethylamine (0.2 mL, 1.42 mmol), cyclopropylacetaldehyde (288.0 mg, 1.92 mmol), and sodium cyanoborohydride (59.2 mg, 0.895 mmol) at 25° C. After stirring for 12 h, the mixture was concentrated in vacuo and the residue was dissolved in ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and concentrated in vacuo. The crude material was purified by flash column chromatography (Teledyne Isco RediSep Flash Column; 0-50% ethyl acetate in hexanes) to afford cis-2-(2-cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester as a yellowish oil (42.7 mg, 0.189, 15%) and trans-2-(2-cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester as a yellowish oil (130.5 mg, 0.579 mmol, 45%). cis-2-(2-Cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester: 1H NMR (400 MHz, CDCl3) δ 0.08-0.12 (2H, m), 0.45-0.49 (2H, m), 0.63-0.72 (1H, m), 1.29 (3H, t, J=7.0 Hz), 1.46-1.52 (2H, m), 1.58-1.77 (2H, m), 1.85-2.10 (4H, m), 2.73-2.87 (2H, m), 3.03 (1H, q, J=6.7 Hz), 3.36 (1H, q, J=7.3 Hz), 4.17 (2H, q, J=7.0 Hz). LC-MS (ESI) calcd for C13H23NO2 225.17, found 226.2 [M+H+]. trans-2-(2-Cyclopropylethylamino)-cyclopentanecarboxylic acid ethyl ester: 1H NMR (400 MHz, CDCl3) δ 0.12-0.16 (2H, m), 0.50-0.55 (2H, m), 0.65-0.72 (1H, m), 1.31 (3H, t, J=7.1 Hz), 1.53-1.59 (2H, m), 1.64-1.84 (2H, m), 1.89-2.13 (4H, m), 2.81-2.87 (1H, m), 2.95-3.01 (1H, m), 3.07 (1H, q, J=7.1 Hz), 3.44 (1H, q, J=7.2 Hz), 4.20 (2H, q, J=7.0 Hz). LC-MS (ESI) calcd for C13H23NO2 225.17, found 226.2 [M+H+].

후처리

  1. concentrationthe mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by flash column chromatography (Teledyne Isco RediSep Flash Column; 0-50% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-2ccdab956d3d458994740f7a4b899808
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582626B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트