Potassium Phosphate, Tribasic → HCID 66890005、化合物

HRID 1897948ノート

反応式

HRID 1897948 の反応式
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]

参加物

6

反応物 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、化合物

生成物 1

HCID 66890005HCID 66890005、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-86ba5546b46640bf878d1da41f3c14cb
出典データセット
uspto-grants-2013_08
特許番号
US08519136B2

反応ノート

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