HCID 178478629, 화합물 → HCID 178528074, 화합물

HRID 411781노트

반응식

HRID 411781 반응식
[C:1]1([Li])[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12.[Cl-].[Cl-].[Cl-].C1([Zr+3:26])C=CC=C1>C1(C)C=CC=CC=1.C(OCC)C>[C:1]1([Zr:26])[CH:16]=[CH:15][CH:14]=[C:13]2[C:2]=1[CH:3]=[C:4]1[C:12]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[N:6]=[C:5]12

참가 물질

5

반응물 2

HCID 178478629HCID 178478629, 화합물HCID 178506658HCID 178506658, 화합물

생성물 1

HCID 178528074HCID 178528074, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매2회HCID 3283Diethyl Ether용매2회

실험 절차

A sample of the indeno[1 2-b]indolyl lithium salt produced above (10 g, 42 mmol) is dissolved in toluene (95 mL) to produce an orange slurry. Diethyl ether (35 mL) is added slowly to give an orange solution. This solution is added over 15 min. at room temperature with stirring to a slurry of cyclopentadienylzirconium trichloride (11 g, 42 mmol) in toluene (190 mL) and diethyl ether (190 mL). The mixture turns deep red and is kept at room temperature overnight. The slurry is filtered to recover a red solid, which is washed with toluene (200 mL) and dried under vacuum. Yield of complex 10: 16.5 g. The 1H NMR spectrum is consistent with the proposed structure:

후처리

  1. customto produce an orange slurry
  2. customto give an orange solution
  3. additionThis solution is added over 15 min. at room temperature
  4. filtrationThe slurry is filtered
  5. customto recover a red solid, which
  6. washis washed with toluene (200 mL)
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-7c5930c9bdd44d4aa67a504df3453fe2
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559251B1

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