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Triethylamine → HCID 178453655, 화합물

HRID 1159362
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HRID 1159362 반응식
CC(OC(OC(OC(C)(C)C)=O)=O)(C)C.C[N:17]([CH2:25][C@H:26]1[CH2:29][C@H:28]([O:30]C2C=CC(CN3CCCC3)=CC=2)[CH2:27]1)[C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21].NC[C@@H]1C[C@H](O)C1.CCN(CC)CC>C1COCC1>[OH:30][C@@H:28]1[CH2:29][C@H:26]([CH2:25][NH:17][C:18](=[O:24])[O:19][C:20]([CH3:22])([CH3:21])[CH3:23])[CH2:27]1
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonateHCID 178484147HCID 178484147, 화합물HCID 178511298HCID 178511298, 화합물

생성물 1

HCID 178453655HCID 178453655, 화합물수율 77%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

(Boc)2O (4.42 g, 0.02 mol) was added to a solution of intermediate 9, cis-3-(aminomethyl)cyclobutanol (1.95 g, 0.019 mol) and Et3N (5.6 mL, 0.039 mol) in 20 mL absolute THF under stirring. The mixture was stirred at room temperature for 30 min, evaporated, and coevaporated with CCl4. The residue was recrystallized form ether to give the title compound (3 g, 77%) as yellow crystals. 1H NMR-data (DMSO-d6): 6.61-6.87 (m, 1H, NH); 4.85 (br.s, 1H, OH); 3.77-3.92 (m, 1H); 2.90 (t, 2H, CH2, J=6.1 Hz); 2.10-2.22 (m, 2H); 1.67-1.80 (m, 1H); 1.21-1.51 (m, 11H, CH2, Boc).

후처리

  1. stirringThe mixture was stirred at room temperature for 30 min
  2. customevaporated
  3. customThe residue was recrystallized form ether

출처 및 근거

ORD 기록
ord-4637e6dbb2844822aebf761cd1d20019
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07812040B2

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