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Hydrochloric Acid → 2-(10,11-Dihydro-dibenzo[a,d]cyclohepten-5-ylidenemethyl)-phenylboronic acid

HRID 2218716
노트
인쇄 미리보기

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HRID 2218716 반응식
[Li]CCCC.Br[C:7]1[CH:28]=[CH:27][CH:26]=[CH:25][C:8]=1[CH:9]=[C:10]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[CH2:14][CH2:13][C:12]2[CH:21]=[CH:22][CH:23]=[CH:24][C:11]1=2.[B:29](OC(C)C)([O:34]C(C)C)[O:30]C(C)C.Cl>C1COCC1>[CH:21]1[C:12]2[CH2:13][CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[C:10](=[CH:9][C:8]3[CH:25]=[CH:26][CH:27]=[CH:28][C:7]=3[B:29]([OH:34])[OH:30])[C:11]=2[CH:24]=[CH:23][CH:22]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 21531Triisopropyl borateHCID 597701175-(2-bromo-benzylidene)-10,11-dihydro-5H-dibenzo[a,d]cyclohepteneHCID 178418339Butyllithium

생성물 1

HCID 597702652-(10,11-Dihydro-dibenzo[a,d]cyclohepten-5-ylidenemethyl)-phenylboronic acid

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
-78 °C

실험 절차

Add n-BuLi (1.6M in hexanes, 12.98 Ml, 20.76 mmol) portionwise (exothermic) to a solution of 5-(2-bromo-benzylidene)-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (5.00 g, 13.84 mmol) in dry THF (50 Ml) at −78° C. under N2. Let stir at −78° C. for 30 min, then add triisopropyl borate (5.21 g, 27.68 mmol) and warm up to room temperature overnight. Add 50 Ml 1.00N HCl and stir for 15 min. Extract into ethyl acetate, dry (MgSO4) and concentrate organics to a brown foam. Recrystallize from boiling hexanes, then chromatograph on silica gel (40 g), eluting with 20% to 50% ethyl acetate/hexanes to afford the title compound as a white foam, mp 134.1° C. MS (ES) 325 (M−H); HPLC shows 82% purity.

후처리

  1. stirringstir for 15 min
  2. extractionExtract into ethyl acetate
  3. dry with materialdry (MgSO4)
  4. concentrationconcentrate organics to a brown foam
  5. customRecrystallize
  6. washchromatograph on silica gel (40 g), eluting with 20% to 50% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-d113203c8ca34e238d0b0a89847b6841
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07411072B2

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