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Hydrochloric Acid → HCID 178444366, 화합물

HRID 2268102
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HRID 2268102 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.B(OC)(OC)OC.Cl.B(O)(O)O.[CH2:25]([C@H:30]1[CH2:35][CH2:34][C@H:33]([C:36]2[CH:41]=[C:40]([F:42])[C:39](I)=[C:38]([F:44])[CH:37]=2)[CH2:32][CH2:31]1)[CH2:26][CH2:27][CH2:28][CH3:29].C(C1CCC(=O)CC1)CCCC.FC1C=C([Mg]Br)C=C(F)C=1.[Li]CCCC.II.C([O-])([O-])=O.[Na+].[Na+]>C1COCC1.C1COCC1.CN(CCN(C)C)C.C1(C)C=CC=CC=1.O>[CH2:25]([C@H:30]1[CH2:35][CH2:34][C@H:33]([C:36]2[CH:37]=[C:38]([F:44])[C:39]([C:2]3[CH:7]=[CH:6][C:5]([O:8][C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=3)=[C:40]([F:42])[CH:41]=2)[CH2:32][CH2:31]1)[CH2:26][CH2:27][CH2:28][CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

15

반응물 10

HCID 313Hydrochloric AcidHCID 807IodineHCID 7628Boric AcidHCID 8470Trimethyl borateHCID 10340Sodium CarbonateHCID 5210081-Bromo-4-(trifluoromethoxy)benzeneHCID 5660974-Pentylcyclohexanone
HCID 178418339
Butyllithium
HCID 178444369HCID 178444369, 화합물
HCID 178505930HCID 178505930, 화합물

생성물 1

HCID 178444366HCID 178444366, 화합물

시약·촉매·용매 4

HCID 962Water용매HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매3회HCID 86588997Thf tmeda용매

실험 절차

A solution of 0.1 mol of p-bromotrifluoromethoxybenzene in 100 ml of THF is added dropwise to a suspension of 0.1 mol of Mg turnings in 50 ml of THF at such a rate that the reaction mixture boils gently. After the mixture has been stirred for one hour, 0.1 mol of trimethyl borate is added dropwise at room temperature, and the mixture is stirred for a further hour and hydrolyzed using dilute hydrochloric acid. After extractive work-up, the resultant boric acid (0.05 mol) is refluxed for two hours together with 0.05 mol of 4-(trans-4-n-pentyl-cyclohexyl)-2,6-difluoroiodobenzene [obtainable by reacting 4-pentylcyclohexanone with 3,5-difluorophenylmagnesium bromide, eliminating water, and hydrogenating the cyclohexylbenzenes on Pd/C. The resultant 3,5-difluoropenyl [sic] compound is metallated at −70° in THF/TMEDA using n-BuLi and subsequently reacted with iodine in THF at −70 °], 38 ml of 2 molar aqueous Na2CO3 solution, 0.6 g of tetrakis(triphenylphosphine)palladium-(0) and 75 ml of toluene. Customary aqueous work-up and chromatographic purification give 4-(trans-4-n-pentylcyclohexyl)-2,6-difluoro-4′-trifluoromethoxybiphenyl.

후처리

  1. stirringthe mixture is stirred for a further hour
  2. customCustomary aqueous work-up and chromatographic purification

출처 및 근거

ORD 기록
ord-36aee8062c8f41a497bb95dc1c40f956
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326066B1

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