Triethylamine → HCID 90006117, 화합물

HRID 718742노트

반응식

HRID 718742 반응식
Cl[CH2:2][C:3]([NH:5][CH2:6][C:7]1[N:8]=[C:9]2[C:14](=[C:15]3[C:20]=1[CH:19]=[CH:18][CH:17]=[CH:16]3)[CH:13]=[CH:12][CH:11]=[CH:10]2)=[O:4].[NH:21]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28][NH:27][CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH:13]1[C:14]2[C:9](=[N:8][C:7]([CH2:6][NH:5][C:3](=[O:4])[CH2:2][N:21]3[CH2:32][CH2:31][NH:30][CH2:29][CH2:28][NH:27][CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)=[C:20]3[C:15]=2[CH:16]=[CH:17][CH:18]=[CH:19]3)[CH:10]=[CH:11][CH:12]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 649631,4,7,10-TetraazacyclododecaneHCID 867124842-Chloro-N-(phenanthridin-6-ylmethyl)acetamide

생성물 1

HCID 90006117HCID 90006117, 화합물수율 47.1%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

A solution of the chloro 9 (20.0 mg, 70.2 μmol) in anhydrous CHCl3 (5 mL) was added to a solution of cyclen (48.4 mg, 0.281 mmol) and triethylamine (11.7 μL, 84.2 μmol) in anhydrous CHCl3 (15 mL) under N2 (g). The reaction mixture was heated to reflux under N2 (g) for 23 hours. The reaction mixture was then allowed to cool to room temperature and washed with NaOH (aq) (1.0 M, 3×5 mL) and H2O (3×5 mL). The organic phase was dried over MgSO4, and concentrated under reduced pressure yielding product 10 as a colorless oil (13.9 mg, 47.1%). This procedure follows closely that developed by Gunnlaugsson and coworkers. (Massue et al. Tetrahedron Lett., 2007, 48, 8052-8055).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux under N2 (g) for 23 hours
  3. washwashed with NaOH (aq) (1.0 M, 3×5 mL) and H2O (3×5 mL)
  4. dry with materialThe organic phase was dried over MgSO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7032c9cfaf014cd299a8313934d2b44b
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09194802B2

반응 노트

불러오는 중…