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Water → HCID 70979338, 화합물

HRID 1485466
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HRID 1485466 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][C@@H:13]([CH3:15])[C:12]3=[N:16][N:17]=[C:18]([CH3:19])[N:11]3[C:10]3[CH:20]=[CH:21][C:22](B4OC(C)(C)C(C)(C)O4)=[CH:23][C:9]2=3)=[CH:4][CH:3]=1.Br[C:34]1[CH:35]=[CH:36][C:37](=[O:41])[NH:38][C:39]=1[CH3:40].C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][C@@H:13]([CH3:15])[C:12]3=[N:16][N:17]=[C:18]([CH3:19])[N:11]3[C:10]3[CH:20]=[CH:21][C:22]([C:34]4[CH:35]=[CH:36][C:37](=[O:41])[NH:38][C:39]=4[CH3:40])=[CH:23][C:9]2=3)=[CH:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 27344173-Bromo-6-hydroxy-2-methylpyridineHCID 70979017HCID 70979017, 화합물

생성물 1

HCID 70979338HCID 70979338, 화합물수율 17%

시약·촉매·용매 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

To a solution of (R)-6-(4-chlorophenyl)-1,4-dimethyl-8-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepine (100 mg, 0.22 mmol) in dioxane/water (11 mL, dioxane/water=10:1) was added 5-Bromo-6-methyl-1H-pyridin-2-one (51 mg, 0.27 mmol), cesium carbonate (145 mg, 0.44 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (17 mg, 0.022 mmol) under nitrogen atmosphere. The mixture was stirred and heated to reflux overnight. The mixture was cooled down and poured into water (30 mL) and extracted with ethyl acetate (20 ml×3). The combined organic phase was concentrated, and the residue was purified by HPLC (Mobile phase A: water with 0.05% ammonia solution; Mobile phase B: MeCN; column temperature: 30° C., Gradient: 25-55% B, 15 min) to give (R)-5-(6-(4-chlorophenyl)-1,4-dimethyl-5,6-dihydro-4H-benzo[b][1,2,4]triazolo[4,3-d][1,4]diazepin-8-yl)-6-methylpyridin-2(1H)-one as a white solid (16 mg, 17%).

후처리

  1. temperatureheated
  2. temperatureto reflux overnight
  3. temperatureThe mixture was cooled down
  4. extractionextracted with ethyl acetate (20 ml×3)
  5. concentrationThe combined organic phase was concentrated
  6. customthe residue was purified by HPLC (Mobile phase A: water with 0.05% ammonia solution; Mobile phase B: MeCN; column temperature: 30° C., Gradient: 25-55% B, 15 min)

출처 및 근거

ORD 기록
ord-2c1800b85e944cd2ab8d79f782e64c29
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09422292B2

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