2-(Dicyclohexylphosphino)biphenyl → HCID 59240555、化合物

HRID 42202

反応式

HRID 42202 の反応式
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

参加物

7

反応物 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

生成物 1

HCID 59240555HCID 59240555、化合物

試薬・触媒・溶媒 2

HCID 167845palladium(II) acetate触媒HCID 1140Toluene溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d0271881ab04280b77fec1a26ed43cb
出典データセット
uspto-grants-2013_09
特許番号
US08536168B2

関連ノート

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