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tert-Butyl carbamate → HCID 86669027, 화합물

HRID 2366311
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HRID 2366311 반응식
[Cl:1][C:2]1[C:7]2[S:8][C:9]([C:11]3[C:16]([F:17])=[CH:15][C:14](I)=[CH:13][C:12]=3[Cl:19])=[N:10][C:6]=2[CH:5]=[CH:4][N:3]=1.[C:20](=[O:27])([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[NH2:21].CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2>C1(C)C=CC=CC=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:19][C:12]1[CH:13]=[C:14]([NH:21][C:20](=[O:27])[O:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH:15]=[C:16]([F:17])[C:11]=1[C:9]1[S:8][C:7]2[C:2]([Cl:1])=[N:3][CH:4]=[CH:5][C:6]=2[N:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 77922tert-Butyl carbamateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 86669028HCID 86669028, 화합물

생성물 1

HCID 86669027HCID 86669027, 화합물수율 78.9%

시약·촉매·용매 4

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 962
Water
용매
HCID 1140Toluene용매
HCID 62657Potassium Phosphate, Tribasic용매

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온도
90 °C

실험 절차

A mixture of 4-chloro-2-(2-chloro-6-fluoro-4-iodo-phenyl)thiazolo[5,4-c]pyridine (715 mg, 1.682 mmol), tert-butyl carbamate (394 mg, 3.365 mmol), Pd2(dba)3 (77 mg, 0.084 mmol), and XantPhos (97 mg, 0.168 mmol) in toluene (17 mL) and K3PO4 (2.65 mL, 1.27 M) was heated at 90° C. under nitrogen for 20 hours. The reaction mixture was diluted with water, extracted with EtOAc (2×). The combined organics were dried (Na2SO4), filtered and concentrated. The crude product was purified by silica gel flash chromatography (0-25% EtOAc/hexane) to give the title compound (550 mg, 78.9% yield) as an off-white solid. 1H NMR (400 MHz, CDCl3) δ 8.48 (d, J=5.6 Hz, 1H), 7.95 (d, J=5.6 Hz, 1H), 7.46-7.33 (m, 2H), 6.70 (s, 1H), 1.55 (s, 9H). LCMS (ESI) m/z 414.1 [M+H+].

후처리

  1. extractionextracted with EtOAc (2×)
  2. dry with materialThe combined organics were dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude product was purified by silica gel flash chromatography (0-25% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-0d8962f89040469b829c47b82f7fc0f9
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08697708B2

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