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Tetrahydrofuran → 3-Morpholin-4-yl-1-triisopropylsilanyl-1H-indole

HRID 1178906
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HRID 1178906 반응식
Br[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([Si:11]([CH:18]([CH3:20])[CH3:19])([CH:15]([CH3:17])[CH3:16])[CH:12]([CH3:14])[CH3:13])[CH:3]=1.[NH:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].C1COCC1>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.C(Cl)(Cl)Cl.[Pd].[Pd].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2N(C)C)CCCCC1>[N:21]1([C:2]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[N:4]([Si:11]([CH:18]([CH3:20])[CH3:19])([CH:15]([CH3:17])[CH3:16])[CH:12]([CH3:14])[CH3:13])[CH:3]=2)[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1
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참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 8083MorpholineHCID 2733832Lithium hexamethyldisilazaneHCID 109917693-Bromo-1-(triisopropylsilyl)indole

생성물 1

HCID 589751763-Morpholin-4-yl-1-triisopropylsilanyl-1H-indole수율 60%

시약·촉매·용매 2

HCID 2734217
2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl
촉매
HCID 11029508Palladium, tris[mu-[(1,2-eta:4,5-eta)-(1E,4E)-1,5-diphenyl-1,4-pentadien-3-one]]di-, compd. with trichloromethane (1:1)촉매

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온도
65 °C

실험 절차

Combine 3-bromo-1-triisopropylsilanyl-1H-indole (0.33 g, 0.94 mmol), morpholine (0.10 mL, 1.15 mmol), 2-dicyclohexylphosphino-2′-(N,N-dimethylamino)biphenyl (0.012 g, 0.03 mmol), and tris(dibenzylideneacetone)dipalladium(0) chloroform adduct (0.012 g, 0.01 mmol) in a pressure tube. Add 1N solution of lithium bis(trimethylsilyl)amide in THF (2.00 mL, 2.00 mmol), flush tube with nitrogen gas, and close the tube. Stir at 65° C. for 18 h, cool to room temperature, dilute with water, and extract with EtOAc. Wash EtOAc layer with water, brine, dry (Na2SO4), and concentrate under vacuum. Purify the residue by flash chromatography using 0 to 50% of EtOAc in hexanes to give the title compound (0.20 g 60%): MS (ES) 359.1 (M+1)+.

후처리

  1. customflush tube with nitrogen gas
  2. customclose the tube
  3. temperaturecool to room temperature
  4. additiondilute with water
  5. extractionextract with EtOAc
  6. dry with materialWash EtOAc layer with water, brine, dry (Na2SO4)
  7. concentrationconcentrate under vacuum
  8. customPurify the residue by flash chromatography

출처 및 근거

ORD 기록
ord-4fd79a99684e4282aaaad65ec6a8280a
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07276516B2

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