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Toluene → HCID 11662049, 화합물

HRID 1432172
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HRID 1432172 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8]2[C:9]3[C:16]4[CH2:17][CH2:18][CH2:19][CH2:20][C:15]=4[S:14][C:10]=3[N:11]=[CH:12][N:13]=2)[CH2:3][CH2:2]1.[F:21][C:22]1[CH:23]=[C:24]([CH2:28][C:29](C2C=CC=CC=2)=O)[CH:25]=[CH:26][CH:27]=1.[C-:37]#[N:38].C([Al+]CC)C.C1(C)C=CC=CC=1>C(Cl)Cl.CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[F:21][C:22]1[CH:23]=[C:24]([C:28]([N:1]2[CH2:2][CH2:3][CH:4]([NH:7][C:8]3[C:9]4[C:16]5[CH2:17][CH2:18][CH2:19][CH2:20][C:15]=5[S:14][C:10]=4[N:11]=[CH:12][N:13]=3)[CH2:5][CH2:6]2)([CH3:29])[C:37]#[N:38])[CH:25]=[CH:26][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 1140TolueneHCID 27590612-(3-fluorophenyl)-1-phenylethanoneHCID 16686413Diethyl aluminum cyanideHCID 22182391HCID 22182391, 화합물

생성물 1

HCID 11662049HCID 11662049, 화합물수율 100%

시약·촉매·용매 2

HCID 11026
Titanium isopropoxide
촉매
HCID 6344Dichloromethane용매

실험 절차

To a mixture of N-(piperidin-4-yl)-5,6,7,8-tetrahydro-benzo[4,5]thieno[2,3-d]pyrimidin-4-amine (2.86 g, 10 mmol) and 3-fluorophenylacetophenone (1.38 g, 10 mmol) in dry DCM (25 mL) was added titanium isopropoxide (2.85 g, 10 m.mol) at room temperature and stirred for 24 h. 1 M solution of diethylaluminumcyanide in toluene (1.2 mL, 10 mmol) was added to the above solution and the mixture was allowed to stir for 24 h. The reaction was quenched by the addition of saturated aq. NaHCO3 solution (15 mL) and the organic layer was separated, dried and concentrated under reduced pressure to get the title compound (4.3 g, 100%) as pale yellow powder. 1H NMR (400 MHz, CDCl3): δ 8.01 (s, 1H), 7.35-7.24 (m, 2H), 6.99 (t, 1H), 6.78 (t, 1H), 4.21 (brs, 1H, NH), 3.91-3.86 (m, 1H), 3.11-3.03 (m, 2H), 2.91 (t, 2H), 2.49-2.27 (m, 4H), 2.00-1.92 (m, 4H), 1.42 (s, 3H). MS (ESI) m/z: Calculated: 435.56; Observed: 436.2 (M++1).

후처리

  1. stirringto stir for 24 h
  2. customThe reaction was quenched by the addition of saturated aq. NaHCO3 solution (15 mL)
  3. customthe organic layer was separated
  4. customdried
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-173623c9286f44e1a171a3bd33e6f443
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612078B2

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