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Dimethylformamide → HCID 66933293, 화합물

HRID 449825
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HRID 449825 반응식
[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]1[CH2:20][C:11]2[NH:12][C:13]3[CH:14]=[CH:15][C:16](Br)=[CH:17][C:18]=3[C:10]=2[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[CH3:22][N:23](C=O)C>[C-]#N.[Zn+2].[C-]#N.C([O-])(=O)C.[Zn+2].C([O-])(=O)C.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2].[Pd](Cl)Cl.[Zn]>[C:1]([O:5][C:6](=[O:21])[NH:7][C@@H:8]1[CH2:20][C:11]2[NH:12][C:13]3[CH:14]=[CH:15][C:16]([C:22]#[N:23])=[CH:17][C:18]=3[C:10]=2[CH2:9]1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

8

반응물 2

HCID 6228DimethylformamideHCID 66933350HCID 66933350, 화합물

생성물 1

HCID 66933293HCID 66933293, 화합물수율 69%

시약·촉매·용매 5

HCID 11186Zinc cyanide (Zn(CN)2)촉매HCID 11192Zinc Acetate촉매HCID 23994Zinc촉매
HCID 24290
Palladium Chloride
촉매
HCID 635956Ferrocene-1,1'-bis-(diphenylphosphine)촉매

실험 절차

The following reagents are stirred together in DMF (250 mL) at 100° C. for 18 h: ((S)-7-bromo-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl)-carbamic acid tert-butyl ester (50.0 g, 142 mmol), zinc cyanide (11.9 g, 99.7 mmol), zinc acetate (5.22 g, 28.5 mmol), 1,1′-bis(diphenylphosphino)ferrocene)palladium (II) chloride (Pd(dppf)2Cl2) (1.74 g, 2.14 mmol), and zinc (3.72 g, 56.9 mmol). The reaction is concentrated to dryness and partitioned between water and ethyl acetate. The organics are washed with water and brine, then concentrated to afford a solid. The solid is chromatographed in two equal portions on silica gel (1600 mL) as follows: load as a solution in CH2Cl2 and elute with 2% EtOAc in CH2Cl2 (3 L), then 5% EtOAc in CH2Cl2. The product is recovered from the two columns to give 29 g (69%) of the title compound as a white solid. 1H-NMR (400 MHz, CDCl3) δ 8.39 (s, 1H), 7.74 (s, 1H), 7.34 (d, J=1.8 Hz, 2H), 5.05-4.96 (m, 2H), 3.37-3.25 (m, 2H), 2.80-2.63 (m, 2H), 1.46 (s, 9H).

후처리

  1. concentrationThe reaction is concentrated to dryness
  2. custompartitioned between water and ethyl acetate
  3. washThe organics are washed with water and brine
  4. concentrationconcentrated
  5. customto afford a solid
  6. customThe solid is chromatographed in two equal portions on silica gel (1600 mL)
  7. washload as a solution in CH2Cl2 and elute with 2% EtOAc in CH2Cl2 (3 L)
  8. customThe product is recovered from the two columns

출처 및 근거

ORD 기록
ord-7d4ee2a6a9d3414a8e28b85dd9afdf6f
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08486943B2

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