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Hydrochloric Acid → HCID 71698376, 화합물

HRID 539898
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HRID 539898 반응식
[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH:11][C:12]3[N:17]=[C:16]([N:18]4[CH:22]=[C:21]([CH:23]=O)[C:20]([CH3:25])=[N:19]4)[CH:15]=[CH:14][N:13]=3)[CH:9]=2)[N:4]([CH3:26])[C:3]=1[CH3:27].Cl.C([N:31]([CH2:34][CH3:35])[CH2:32]C)C.[BH-](OC(C)=O)(OC(C)=O)[O:37]C(C)=O.[Na+]>ClCCl>[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH:11][C:12]3[N:17]=[C:16]([N:18]4[CH:22]=[C:21]([CH2:23][N:31]5[CH2:32][CH:35]([OH:37])[CH2:34]5)[C:20]([CH3:25])=[N:19]4)[CH:15]=[CH:14][N:13]=3)[CH:9]=2)[N:4]([CH3:26])[C:3]=1[CH3:27]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 866989881-(2-(3-chloro-1,2-dimethyl-1H-indol-5-ylamino)pyrimidin-4-yl)-3-methyl-1H-pyrazole-4-carbaldehyde

생성물 1

HCID 71698376HCID 71698376, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

To a slurry of Intermediate No. 9 (642 mg, 1.68 mmol), 3-azetidinole hydrochloride (370 mg, 2 equiv.) and triethylamine (1.4 mL, 6 equiv.) in 100 mL of dichloromethane, was added NaBH(OAc)3 (1.07 g, 3 equiv.) at room temperature. The reaction was stirred for 12 hour at room temperature and then quenched with 1N—NaOH. It was extracted with ethyl acetate and washed twice with brine. The collected organic layer was dried over anhydrous sodium sulfate and then concentrated in vacuo. The resulting residue was purified by silica gel chromatography (DCM/MeOH) to afford desired Compound No. 141 as a pale yellow solid (540 mg, 73%); MS (ESI) m/z 438 [M+H]+; 1H NMR (300 MHz, DMSO-d3) δ 9.72 (s, 1H), 8.59 (s, 1H), 8.52 (d, 1H, J=5.4 Hz), 7.95 (s, 1H), 7.45 (s, 2H), 7.14 (s, 1H, J=5.4 Hz), 4.41 (m, 1H), 4.05 (m, 4H), 3.70 (s, 3H), 3.35 (m, 2H), 2.42 (s, 3H), 2.34 (s, 3H).

후처리

  1. customquenched with 1N—NaOH
  2. extractionIt was extracted with ethyl acetate
  3. washwashed twice with brine
  4. dry with materialThe collected organic layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by silica gel chromatography (DCM/MeOH)

출처 및 근거

ORD 기록
ord-1f049c1d44d343ddbfaebc3dfba37e86
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871778B2

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