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Potassium Phosphate, Tribasic → HCID 86630875, 화합물

HRID 17553
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HRID 17553 반응식
P([O-])([O-])([O-])=O.[K+].[K+].[K+].[NH2:9][C:10]1[C:17]([N+:18]([O-:20])=[O:19])=[C:16]([N:21]2[CH2:25][CH2:24][C@H:23]([N:26]([CH3:28])[CH3:27])[CH2:22]2)[C:15](Br)=[C:14]([CH3:30])[C:11]=1[C:12]#[N:13].[C:31]1(B(O)O)[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O1CCOCC1>[NH2:9][C:10]1[C:17]([N+:18]([O-:20])=[O:19])=[C:16]([N:21]2[CH2:25][CH2:24][C@H:23]([N:26]([CH3:28])[CH3:27])[CH2:22]2)[C:15]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:14]([CH3:30])[C:11]=1[C:12]#[N:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 66827Phenylboronic AcidHCID 866308742-Amino-5-bromo-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-3-nitrobenzonitrile

생성물 1

HCID 86630875HCID 86630875, 화합물수율 90.2%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물
촉매
HCID 312751,4-Dioxane용매

실험 절차

Potassium phosphate (115 mg, 0.54 mmol) and Pd(PPh3)4 (16 mg, 5 mol %) were added to a dioxane (3 ml) solution of 2-amino-5-bromo-4-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-methyl-3-nitrobenzonitrile (I-267) (100 mg, 0.27 mmol) and phenylboronic acid (40 mg, 0.33 mmol), followed by purging with nitrogen and heating under reflux for 18 hours. After cooling, water was added, followed by extraction with ethyl acetate. The organic layer was washed with saturated brine, then dried over anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the residue was subjected to column chromatography, and eluted with a mixed solvent of chloroform/methanol (2:1, v/v) to obtain the entitled compound (89 mg, 90%) as a dark red solid.

후처리

  1. customby purging with nitrogen
  2. temperatureheating
  3. temperatureunder reflux for 18 hours
  4. temperatureAfter cooling
  5. additionwater was added
  6. extractionfollowed by extraction with ethyl acetate
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe solvent was evaporated away under reduced pressure
  10. washeluted with a mixed solvent of chloroform/methanol (2:1

출처 및 근거

ORD 기록
ord-84f4ddda690b40b8a02f0582e27a5e7a
출처 데이터셋
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07737166B2

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