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Ethanolamine → (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-hydroxyethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide

HRID 505753
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HRID 505753 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:10]2[C@@H:18]([CH:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)[C@@H:17]3[C:12]([C:13]4[CH:27]=[CH:26][C:25]([C:28]([OH:30])=O)=[CH:24][C:14]=4[CH2:15][CH2:16]3)=[N:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9].ON1C2C=CC=CC=2N=N1.C(N(CC)CC)C.F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.[CH2:70]([CH2:72][NH2:73])[OH:71]>CN(C)C=O.C(#N)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([N:10]2[C@@H:18]([CH:19]3[CH2:23][CH2:22][CH2:21][CH2:20]3)[C@@H:17]3[C:12]([C:13]4[CH:27]=[CH:26][C:25]([C:28]([NH:73][CH2:72][CH2:70][OH:71])=[O:30])=[CH:24][C:14]=4[CH2:15][CH2:16]3)=[N:11]2)[CH:5]=[CH:6][C:7]=1[C:8]#[N:9]
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참가 물질

8

반응물 5

HCID 700EthanolamineHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 46871935Pf-03882845

생성물 1

HCID 66722897
(3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-hydroxyethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide
수율 33%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 18373917Acetonitrile--water (1/1)용매

실험 절차

To a solution of (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxylic acid, Example 15 (90 mg, 0.20 mmol) in N,N-dimethylformamide (1 mL) was added 1-hydroxybenzotriazole (43 mg, 0.32 mmol), triethylamine (0.06 mL, 0.40 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium tetrafluoroborate (103 mg, 0.32 mmol). The solution was stirred for twenty-five minutes followed by addition of ethanolamine (0.02 mL, 0.32 mmol). The solution was stirred for twenty hours at ambient temperature. The reaction was quenched with water and the resulting yellow solid was collected by vacuum filtration. Chromatography (reverse phase, acetonitrile/water) provided (3S,3aR)-2-(3-chloro-4-cyanophenyl)-3-cyclopentyl-N-(2-hydroxyethyl)-3,3a,4,5-tetrahydro-2H-benzo[g]indazole-7-carboxamide (yellow solid, 30 mg, 33% yield). LC/MS on 4.6×50 mm C-18 column, tR=6.00 minutes (10 to 90% acetonitrile/water over 6 minutes at 2 mL/minute with detection 254 nm, at 50° C.); ES-MS m/z 463 (M+H); HRMS Calculated for C26H27ClN4O2: 463.1895 (M+H)+. Found: 463.1875; 1H NMR (400 MHz, DMSO-d6) δ ppm 1.10-1.50 (m, 6H), 1.66-1.84 (m, 2H), 2.17-2.25 (m, 1H), 2.87-2.93 (m, 1H), 2.99-3.06 (m, 1H), 3.26-3.34 (m, 2H), 3.48 (t, J=6.18 Hz, 2H), 3.53-3.63 (m, 2H), 4.92 (dd, J=9.13, 6.18 Hz, 1H), 7.17 (dd, J=8.46, 1.75 Hz, 1H), 7.38 (d, J=2.15 Hz, 1H), 7.65 (d, J=8.86 Hz, 1H), 7.73 (d, J=8.59 Hz, 1H), 7.76 (s, 1H), 8.03 (d, J=8.06 Hz, 1H), 8.46 (t, J=6.31 Hz, 1H).

후처리

  1. stirringThe solution was stirred for twenty hours at ambient temperature
  2. customThe reaction was quenched with water
  3. filtrationthe resulting yellow solid was collected by vacuum filtration

출처 및 근거

ORD 기록
ord-1c4855b0c0064751af85b6dd33042ee9
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781428B2

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