Diisopropylethylamine → 2-[2-(3-Trifluoromethyl-4,5,6,7-tetrahydroindazol-1-yl)-acetylamino]-4,5,6,7-tetrahydro-benzo[b]thiophene-3-carboxylic acid tert-butyl ester
반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]([CH2:12][C:13]([OH:15])=O)[N:4]=1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.CCN(C(C)C)C(C)C.[C:51]([O:55][C:56]([C:58]1[C:59]2[CH2:67][CH2:66][CH2:65][CH2:64][C:60]=2[S:61][C:62]=1[NH2:63])=[O:57])([CH3:54])([CH3:53])[CH3:52]>CN(C=O)C.C(Cl)Cl>[C:51]([O:55][C:56]([C:58]1[C:59]2[CH2:67][CH2:66][CH2:65][CH2:64][C:60]=2[S:61][C:62]=1[NH:63][C:13](=[O:15])[CH2:12][N:5]1[C:6]2[CH2:7][CH2:8][CH2:9][CH2:10][C:11]=2[C:3]([C:2]([F:1])([F:17])[F:16])=[N:4]1)=[O:57])([CH3:54])([CH3:52])[CH3:53]참가 물질
7
반응물 4
HCID 81531Diisopropylethylamine
HCID 788039[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]acetic acid
HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
HCID 10777280tert-Butyl 2-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-3-carboxylate생성물 1
시약·촉매·용매 2
실험 절차
(3-Trifluoromethyl-4,5,6,7-tetrahydroindazol-1-yl)-acetic acid (638 mg, 2.57 mmol) was suspended in a solution of DCM (10 mL) and DMF (1 mL) and O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (1.17 g, 3.08 mmol) and N,N′-diisopropylethylamine (537 μL, 3.08 mmol) added, followed by 2-Amino-4,5,6,7-tetrahydro-benzo[b]thiophene-3-carboxylic acid tert-butyl ester (651 mg, 2.57 mmol). The resultant mixture was stirred at RT overnight. The solution was concentrated in vacuo. The residue was purified by silica gel chromatography using DCM as eluent, to afford the title compound as a yellow solid (0.93 g, 1.93 mmol, 75%).
후처리
- additionadded
- concentrationThe solution was concentrated in vacuo
- customThe residue was purified by silica gel chromatography
출처 및 근거
- ORD 기록
- ord-95ccfd06898a450abfd5b508ffb59f9a
- 출처 데이터셋
- uspto-grants-2010_10
- 특허 번호
- US07820707B2
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