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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Chloroform → Benzenamine, 4-(1-methyl-2-pyrrolidinyl)-

HRID 2236496
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HRID 2236496 반응식
[Li+].C[Si]([N-:6][Si](C)(C)C)(C)C.C(Cl)(Cl)Cl.P(C(C)(C)C)(C(C)(C)C)C(C)(C)C.[H+].[B-](F)(F)(F)F.Br[C:35]1[CH:40]=[CH:39][C:38]([CH:41]2[CH2:45][CH2:44][CH2:43][N:42]2[CH3:46])=[CH:37][CH:36]=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.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[CH3:46][N:42]1[CH2:43][CH2:44][CH2:45][CH:41]1[C:38]1[CH:39]=[CH:40][C:35]([NH2:6])=[CH:36][CH:37]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 6212ChloroformHCID 28118Tetrafluoroboric acidHCID 83681Tris(1,1-dimethylethyl)phosphineHCID 2848972-(4-Bromophenyl)-1-methylpyrrolidineHCID 2733832Lithium hexamethyldisilazane

생성물 1

HCID 59300155Benzenamine, 4-(1-methyl-2-pyrrolidinyl)-

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 1140Toluene용매

실험 절차

LiHMDS (5.0 g, 30.0 mmol) is added to a 250 mL round bottom flask. Toluene (60 mL) is then added followed by addition of Pd2(dba)3.CHCl3 (390 mg, 0.39 mmol) and P(tBu)3.HBF4 (300 mg, 1.03 mmol) and 2-(4-Bromo-phenyl)-1-methyl-pyrrolidine (3.5 g, 14.5 mmol). The mixture is degassed. The resulting mixture is then stirred at room temperature overnight. After TLC suggested no starting bromide left, the reaction mixture is diluted with ether and poured into dilute HCl (aq). The ether layer is discarded, the aqueous layer is basified with NH4OH and extracted with CH2Cl2. The CH2Cl2 layer is dried and concentrated. The residue is judged by NMR to be 90% purity product (2.52 g, 90%).

후처리

  1. customThe mixture is degassed
  2. waitleft
  3. additionthe reaction mixture is diluted with ether
  4. additionpoured into dilute HCl (aq)
  5. extractionextracted with CH2Cl2
  6. dry with materialThe CH2Cl2 layer is dried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3f9ccca18cb041fd89fb8aabf9475d6d
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07713994B2

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