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Triethylamine → HCID 57791847, 화합물

HRID 1091713
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HRID 1091713 반응식
Cl.[CH:2]([O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)([CH3:4])[CH3:3].C(N(CC)CC)C.[O:19]=[C:20]1[C:29]2[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:23]([CH2:30][C:31]2[CH:36]=[CH:35][N:34]=[C:33]([C:37](O)=[O:38])[CH:32]=2)=[N:22][NH:21]1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1>CN(C)C=O>[CH3:3][CH:2]([O:5][CH:6]1[CH2:11][CH2:10][N:9]([C:37]([C:33]2[CH:32]=[C:31]([CH2:30][C:23]3[C:24]4[C:29](=[CH:28][CH:27]=[CH:26][CH:25]=4)[C:20](=[O:19])[NH:21][N:22]=3)[CH:36]=[CH:35][N:34]=2)=[O:38])[CH2:8][CH2:7]1)[CH3:4]
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6

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HCID 8471Triethylamine2회HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 509880984-Isopropoxypiperidine hydrochlorideHCID 59767737HCID 59767737, 화합물

생성물 1

HCID 57791847HCID 57791847, 화합물수율 59.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
25 °C

실험 절차

A solution of 4-isopropoxypiperidine hydrochloride (192 mg, 1.07 mmol) and triethylamine (0.327 mL, 2.35 mmol) in N,N-dimethylformamide (3 mL) was added in one portion to a stirred solution of 4-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)picolinic acid (5)(300 mg, 1.07 mmol), triethylamine (0.327 mL, 2.35 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetra-methyluronium hexafluorophosphate (607 mg, 1.60 mmol) in DMF (3 mL) at 25° C. The resulting solution was stirred at 25° C. for 4 hours. The crude mixture was purified by preparative HPLC (Waters XBridge Prep C18 OBD column, 5μ silica, 30 mm diameter, 100 mm length), using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness and lyophilised to afford the desired compound as a solid (257 mg, 59.3%); 1H NMR (400.132 MHz, DMSO) δ 1.08 (6H, dd), 1.28-1.46 (2H, m), 1.65-1.74 (1H, m), 1.78-1.87 (1H, m), 3.12 (1H, ddd), 3.23-3.31 (1H, m), 3.42-3.51 (1H, m), 3.62 (1H, m), 3.69 (1H, quintet), 3.91-4.00 (1H, m), 4.40 (2H, s), 7.39 (1H, dd), 7.49 (1H, d), 7.83-7.97 (3H, m), 8.28 (1H, dd), 8.46-8.49 (1H, m), 12.60 (1H, s); m/z (LC-MS, ESI+), RT=1.54 (M+H 407).

후처리

  1. customThe crude mixture was purified by preparative HPLC (Waters XBridge Prep C18 OBD column, 5μ silica, 30 mm diameter, 100 mm length)
  2. additionFractions containing the desired compound
  3. customwere evaporated to dryness

출처 및 근거

ORD 기록
ord-6c25459a0d154ca5a9f3491557fd58b3
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08129380B2

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