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5-Bromo-1-[tert-butyl(dimethyl)silyl]-1H-indole → HCID 59381924, 화합물

HRID 2354567
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HRID 2354567 반응식
CC([O-])(C)C.[Na+].Br[C:8]1[CH:9]=[C:10]2[C:14](=[CH:15][CH:16]=1)[N:13]([Si:17]([C:20]([CH3:23])([CH3:22])[CH3:21])([CH3:19])[CH3:18])[CH:12]=[CH:11]2.[C:24]([O:28][C:29]([N:31]1[CH2:36][CH2:35][NH:34][CH:33]([CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[CH2:32]1)=[O:30])([CH3:27])([CH3:26])[CH3:25]>C1(C)C(C)=CC=CC=1.C(OCC)(=O)C.CC([O-])=O.CC([O-])=O.[Pd+2].P(C(C)(C)C)(C(C)(C)C)C(C)(C)C>[C:24]([O:28][C:29]([N:31]1[CH2:36][CH2:35][N:34]([C:8]2[CH:9]=[C:10]3[C:14](=[CH:15][CH:16]=2)[N:13]([Si:17]([C:20]([CH3:23])([CH3:22])[CH3:21])([CH3:19])[CH3:18])[CH:12]=[CH:11]3)[CH:33]([CH2:37][C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=2)[CH2:32]1)=[O:30])([CH3:27])([CH3:25])[CH3:26]
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참가 물질

8

반응물 3

HCID 114723735-Bromo-1-[tert-butyl(dimethyl)silyl]-1H-indoleHCID 23676156Sodium t-butoxideHCID 44118664tert-Butyl 3-benzylpiperazine-1-carboxylate

생성물 1

HCID 59381924HCID 59381924, 화합물수율 74.1%

시약·촉매·용매 4

HCID 83681Tris(1,1-dimethylethyl)phosphine촉매
HCID 167845
palladium(II) acetate
촉매
HCID 7237O-Xylene용매3회
HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

To a mixture of Pd(OAc)2 (0.054 g, 0.2 mmol), NaOtBu (0.64 g, 6.6 mmol) in xylene (7.0 mL) in a screw-capped tube was added tBu3P (0.049 g, 0.2 mmol). After 10 minutes a solution of 5-bromo-1-(tert-butyl-dimethyl-silanyl)-1H-indole (1.30 g, 4.4 mmol) in xylene (7.0 mL) and a solution of 3-benzyl-piperazine-1-carboxylic acid tert-butyl ester (1.34 g, 4.8 mmol) in xylene (8.0 mL) were added. The mixture was heated to 80° C. for 30 minutes, then cooled to room temperature. The reaction mixture was taken up in ethyl acetate, filtered through a pad of celite, and concentrated under reduced pressure. Purification via flash chromatography (gradient: 2% to 20% EtOAc in hexane) afforded 3-Benzyl-4-[1-(tert-butyl-dimethyl-silanyl)-1H-indol-5-yl]-piperazine-1-carboxylic acid tert-butyl ester (1.65 g, 74%) as a pale yellow solid; MS (M+H)=506.

후처리

  1. temperaturecooled to room temperature
  2. filtrationfiltered through a pad of celite
  3. concentrationconcentrated under reduced pressure
  4. customPurification via flash chromatography (gradient: 2% to 20% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-826123f264c64f698585ee43f7cf6ce2
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754721B2

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