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Water → HCID 59596388, 화합물

HRID 2264594
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HRID 2264594 반응식
[CH3:1][NH:2][C:3]1[N:8]=[CH:7][N:6]=[C:5]([O:9][C:10]2[CH:11]=[C:12]3[C:16](=[CH:17][CH:18]=2)[NH:15][CH2:14][CH2:13]3)[CH:4]=1.[C:19]([C:23]1[CH:28]=[CH:27][C:26]([N:29]=[C:30]=[O:31])=[CH:25][CH:24]=1)([CH3:22])([CH3:21])[CH3:20].CCOC(C)=O.O>C1COCC1>[C:19]([C:23]1[CH:28]=[CH:27][C:26]([NH:29][C:30]([N:15]2[C:16]3[C:12](=[CH:11][C:10]([O:9][C:5]4[CH:4]=[C:3]([NH:2][CH3:1])[N:8]=[CH:7][N:6]=4)=[CH:18][CH:17]=3)[CH2:13][CH2:14]2)=[O:31])=[CH:25][CH:24]=1)([CH3:22])([CH3:20])[CH3:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 27356951-Tert-butyl-4-isocyanatobenzeneHCID 67531579HCID 67531579, 화합물

생성물 1

HCID 59596388HCID 59596388, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 70 mg (0.3 mMol) 5-(6-methylamino-pyrimidin-4-yloxy)-2,3-dihydro-indole (Step 21.2) and 70 mg (0.4 mMol) 4-tert.butyl-phenylisocyanat in 2 ml THF is stirred for 75 min at rt. The reaction mixture is dissolved with EtOAc and water, the aqueous layer separated off and extracted twice with EtOAc. The organic phases are washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; EtOAc/hexane 1:1→3:1→4:1) gives the title compound: MS: [M+1]+=418; TLC(EtOAc): Rf=0.20.

후처리

  1. customthe aqueous layer separated off
  2. extractionextracted twice with EtOAc
  3. washThe organic phases are washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-68b26c1447364f159df5325604a29153
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07855215B2

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