Triethylamine → HCID 178453335, 화합물

HRID 1450469노트

반응식

HRID 1450469 반응식
[NH:1]1[C:5]([CH2:6][C:7]2[CH:8]=[C:9]3[C:13](=[CH:14][CH:15]=2)[NH:12][CH:11]=[C:10]3[CH2:16][CH2:17][NH2:18])=[N:4][N:3]=[N:2]1.C(N(CC)CC)C.[O:26](C(OC(C)(C)C)=O)[C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=O>C(Cl)Cl>[C:30]([O:29][C:27]([NH:18][CH2:17][CH2:16][C:10]1[C:9]2[C:13](=[CH:14][CH:15]=[C:7]([CH2:6][C:5]3[NH:1][N:2]=[N:3][N:4]=3)[CH:8]=2)[NH:12][CH:11]=1)=[O:26])([CH3:33])([CH3:32])[CH3:31]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 90495Di-tert-butyl dicarbonateHCID 178510860HCID 178510860, 화합물

생성물 1

HCID 178453335HCID 178453335, 화합물수율 64.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred suspension of 2-(5-tetrazol-5-ylmethyl-1H-indol-3-yl)ethylamine (1.76 g, 7.27 mmol) in dry CH2Cl2 (40 ml) was added triethylamine (1.5 g, 14.9 mmol) and (BOC)2O (1.9 g, 7.3 mmol) and the mixture stirred for 16 h. The solvent was removed under vacuum and the residue chromatographed on silica-gel eluting with EtOH/Et2O/H2O/NH3 (20:60:8:1) to give the title product (1.6 g, 64%); δ (360 MHz, CD3OD) 1.41 (9H, s, 3 of CH3); 2.87 (2H, t, J=7.4 Hz, CH2); 3.30 (2H, t, J=7.4 Hz, CH2); 4.32 (2H, s, CH2); 6.99 (1H, d, J=8.3 Hz, Ar--H); 7.04 (1H, s, Ar--H); 7.26 (1H, d, J=8.3 Hz, Ar--H); 7.49 (1H, s, Ar--H).

후처리

  1. customThe solvent was removed under vacuum
  2. customthe residue chromatographed on silica-gel
  3. washeluting with EtOH/Et2O/H2O/NH3 (20:60:8:1)

출처 및 근거

ORD 기록
ord-a8f3ed208496482abffce2c0e10aacff
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602162

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