2-(Dicyclohexylphosphino)biphenyl → HCID 59240555, 화합물

HRID 42202

반응식

HRID 42202 반응식
Cl[C:2]1[N:7]=[CH:6][C:5]([CH2:8][C:9]([N:11]2[CH2:15][CH2:14][CH2:13][CH2:12]2)=[O:10])=[CH:4][CH:3]=1.[CH2:16]([C:23]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:26]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[N:25][N:24]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C1CCC(P(C2C(C3C=CC=CC=3)=CC=CC=2)C2CCCCC2)CC1.CC([O-])(C)C.[K+]>C1(C)C=CC=CC=1.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH2:16]([C:23]1[C:32]2[C:27](=[CH:28][CH:29]=[CH:30][CH:31]=2)[C:26]([N:33]2[CH2:38][CH2:37][N:36]([C:2]3[N:7]=[CH:6][C:5]([CH2:8][C:9]([N:11]4[CH2:15][CH2:14][CH2:13][CH2:12]4)=[O:10])=[CH:4][CH:3]=3)[CH2:35][CH2:34]2)=[N:25][N:24]=1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

참가 물질

7

반응물 4

HCID 27342162-(Dicyclohexylphosphino)biphenylHCID 64040231-Benzyl-4-piperazin-1-yl-phthalazineHCID 23665647Potassium tert-butoxideHCID 574716142-(6-Chloro-pyridin-3-yl)-1-pyrrolidin-1-yl-ethanone

생성물 1

HCID 59240555HCID 59240555, 화합물

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매HCID 1140Toluene용매

반응 조건

온도
90 °C

실험 절차

To a solution of this amide (0.22 g, 1 mmol) and 1-benzyl-4-piperazin-1-yl-phthalazine (0.15 g, 0.5 mmol) in toluene (10 mL) were added (2-biphenyl)dicyclohexyl phosphine (35 mg, 0.1 mmol), Pd(OAc)2 (11 mg, 0.05 mmol) and KOtBu (336 mg, 3 mmol). The mixture was degassed and then heated in a microwave reactor at 90° C. The reaction mixture was cooled to room temperature and filtered. Water was added to the filtrate and extracted with EtOAc. The combined organic layers were washed with water, sat. NaHCO3, brine, dried over Na2SO4, filtered and concentrated.

후처리

  1. customThe mixture was degassed
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationfiltered
  4. additionWater was added to the filtrate
  5. extractionextracted with EtOAc
  6. washThe combined organic layers were washed with water, sat. NaHCO3, brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3d0271881ab04280b77fec1a26ed43cb
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536168B2

연결된 노트

불러오는 중…