Trifluoroacetic acid → HCID 136381126, 화합물

HRID 53581노트

반응식

HRID 53581 반응식
C(OCC1CSC2N(C(=O)C2NC(=O)CC2N=C(C3C=CC=CC=3O)SC=2)C=1C(O)=O)(=O)C.C1(C([O:47][C:48]([C:50]2[N:51]3[CH:54]([S:55][CH2:56][C:57]=2[CH2:58][O:59][C:60](=[O:62])[CH3:61])[CH:53]([NH:63][C:64](=[O:79])[CH2:65][C:66]2[N:67]=[C:68]([C:71]4[C:76]([OH:77])=[CH:75][CH:74]=[CH:73][C:72]=4[OH:78])[S:69][CH:70]=2)[C:52]3=[O:80])=[O:49])C2C=CC=CC=2)C=CC=CC=1.[SiH](CC)(CC)CC.FC(F)(F)C(O)=O>C(Cl)CCl>[C:60]([O:59][CH2:58][C:57]1[CH2:56][S:55][CH:54]2[N:51]([C:52](=[O:80])[CH:53]2[NH:63][C:64](=[O:79])[CH2:65][C:66]2[N:67]=[C:68]([C:71]3[C:76]([OH:77])=[CH:75][CH:74]=[CH:73][C:72]=3[OH:78])[S:69][CH:70]=2)[C:50]=1[C:48]([OH:49])=[O:47])(=[O:62])[CH3:61]

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 136381123HCID 136381123, 화합물HCID 136381127HCID 136381127, 화합물

생성물 1

HCID 136381126HCID 136381126, 화합물수율 88%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

The procedure used for the preparation of 9a was repeated with 8e (181 mg, 0.270 mmol), Et3SiH (0.431 mL, 2.70 mmol), and trifluoroacetic acid (0.832 mL, 10.8 mmol) in dry ClCH2CH2Cl (6 mL) at 0° C. under nitrogen to give 9e (120 mg, 88%) as a white solid after crystallization from EtOAc/CH2Cl2 /hexane. mp 145° C. (dec); IR (KBr) 3650-2500 (br), 1775, 1736, 1466, 1237 cm-1 ; 1H NMR (DMSO-d6) δ1.98 (3H, s, CH3), 3.43 (1H, d, J=18.1 Hz ), 3.58 (1H, d, J=18.1 Hz), 3.76 (2H, s, CH2), 4.64 (1H, d, J=12.8 Hz), 4.95 (1H, d, J=12.8 Hz), 5.05 (1H, d, J=5.0 Hz), 5.64-5.70 (1H, m), 6.42 (2H, d, J=8.0 Hz), 7.07 (1H, t, J=8.0 Hz), 7.41 (1H, s), 9.12 (1H, d, J=8.1 Hz, NH), 12.17 (2H, br s, OH), 13.60 (1H, br s, CO2H); FDMS m/z 505 (M+), 506 (M+ +1); Anal. Calcd for C21H19N3O8S2 : C, 49.89; H, 3.79; N 8.31. Found. C 50.15; H 3.79; N 8.60.

출처 및 근거

ORD 기록
ord-1e7443bcd03e450a892e83141de1c3f7
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05620968

반응 노트

불러오는 중…