Potassium Phosphate, Tribasic → HCID 66890005, 화합물

HRID 1897948노트

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HRID 1897948 반응식
Br[C:2]1[N:7]=[C:6]([CH2:8][C:9]2([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:5]=[CH:4][CH:3]=1.[C:27]([N:31]1[C:35]([NH2:36])=[CH:34][CH:33]=[N:32]1)([CH3:30])([CH3:29])[CH3:28].CC1(C)C2C=CC=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=2OC2C1=CC=CC=2P(C1C=CC=CC=1)C1C=CC=CC=1.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>O1CCOCC1>[C:27]([N:31]1[C:35]([NH:36][C:2]2[N:7]=[C:6]([CH2:8][C:9]3([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]3)[CH:5]=[CH:4][CH:3]=2)=[CH:34][CH:33]=[N:32]1)([CH3:30])([CH3:29])[CH3:28]

참가 물질

6

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 398690981-tert-Butyl-1H-pyrazol-5-amineHCID 86649625HCID 86649625, 화합물

생성물 1

HCID 66890005HCID 66890005, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A mixture of 1.33 g of 1-tert-butyl 4-ethyl 4-((6-bromopyridin-2-yl)methyl)piperidine-1,4-dicarboxylate, 650 mg of 1-tert-butyl-1H-pyrazol-5-amine (WO2007/126126, page 72, Reference 1), 360 mg of 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene, 322 mg of tris(dibenzylideneacetone)dipalladium(0)-chloroform complex, 1.98 g of potassium phosphate and 30 ml of 1,4-dioxane was stirred at 100° C. for 4 hours, followed by cooling down to room temperature. An insoluble matter was filtered off using Celite and washed with ethyl acetate. The resulting ethyl acetate solution was concentrated in vacuo. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=20/1−3/2) to give the title compound as a pale brown oil.

후처리

  1. temperatureby cooling down to room temperature
  2. filtrationAn insoluble matter was filtered off
  3. washwashed with ethyl acetate
  4. concentrationThe resulting ethyl acetate solution was concentrated in vacuo
  5. customThe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate=20/1−3/2)

출처 및 근거

ORD 기록
ord-86ba5546b46640bf878d1da41f3c14cb
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08519136B2

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