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Water → (2s,3s,5r)-2-Benzyl-3-{(3-chloro-5-trifluoromethyl-benzyl)-[5-(1-methyl-1h-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-5-ethyl-pyrrolidine-1-carboxylic acid isopropyl ester

HRID 409429
ノート
印刷プレビュー

反応式

HRID 409429 の反応式
[CH:1]([O:4][C:5]([N:7]1[C@H:11]([CH2:12][CH3:13])[CH2:10][C@H:9]([N:14]([C:27]2[N:32]=[CH:31][C:30](Br)=[CH:29][N:28]=2)[CH2:15][C:16]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[C:18]([Cl:26])[CH:17]=2)[C@@H:8]1[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:6])([CH3:3])[CH3:2].[CH3:41][N:42]1[CH:46]=[C:45](B2OC(C)(C)C(C)(C)O2)[CH:44]=[N:43]1.C(=O)([O-])[O-].[Na+].[Na+].O>COCCOC.[Cl-].[Na+].O.[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH:1]([O:4][C:5]([N:7]1[C@H:11]([CH2:12][CH3:13])[CH2:10][C@H:9]([N:14]([CH2:15][C:16]2[CH:21]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:19]=[C:18]([Cl:26])[CH:17]=2)[C:27]2[N:32]=[CH:31][C:30]([C:45]3[CH:44]=[N:43][N:42]([CH3:41])[CH:46]=3)=[CH:29][N:28]=2)[C@@H:8]1[CH2:34][C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)=[O:6])([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 27739871-Methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazoleHCID 42633349(2S,3S,5R)-2-Benzyl-3-[(5-bromo-pyrimidin-2-yl)-(3-chloro-5-trifluoromethyl-benzyl)-amino]-5-ethyl-pyrrolidine-1-carboxylic acid isopropyl ester

生成物 1

HCID 42633350
(2s,3s,5r)-2-Benzyl-3-{(3-chloro-5-trifluoromethyl-benzyl)-[5-(1-methyl-1h-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-5-ethyl-pyrrolidine-1-carboxylic acid isopropyl ester
収率 51%

試薬・触媒・溶媒 3

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒HCID 80711,2-Dimethoxyethane溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
90 °C

実験手順

(2S,3S,5R)-2-Benzyl-3-[(5-bromo-pyrimidin-2-yl)-(3-chloro-5-trifluoromethyl-benzyl)-amino]-5-ethyl-pyrrolidine-1-carboxylic acid isopropyl ester (0.042 mmol; 27 mg), tetrakis(triphenylphosphine) palladium (0.0042 mmol; 4.9 mg), 1-methylpyrazol-4-boronic acid pinacol ester (0.063 mmol; 13 mg) and sodium carbonate (0.084 mmol; 8.9 mg) are dissolved in 1,2-dimethoxyethane (0.8 mL) and water (0.08 mL) at room temperature. The mixture is stirred at 90° C. for 17 hours, and then cooled to ambient temperature. To the mixture is added brine and the solution is extracted three times with EtOAc. The combined organic layer is washed with brine, dried over Na2SO4, filtered, and concentrated under reduced pressure. The obtained residue is purified by silica gel column chromatography (eluent: n-hexane/EtOAc) to give (2S,3S,5R)-2-Benzyl-3-{(3-chloro-5-trifluoromethyl-benzyl)-[5-(1-methyl-1H-pyrazol-4-yl)-pyrimidin-2-yl]-amino}-5-ethyl-pyrrolidine-1-carboxylic acid isopropyl ester (13.6 mg, 51%); ESI-MS m/z: 641 [M+1]+, Retention time 2.62 min (condition A).

後処理

  1. customat room temperature
  2. temperaturecooled to ambient temperature
  3. extractionthe solution is extracted three times with EtOAc
  4. washThe combined organic layer is washed with brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe obtained residue is purified by silica gel column chromatography (eluent: n-hexane/EtOAc)

出典と根拠

ORDレコード
ord-b0775fece25f4f28a429dca19745adbc
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759365B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート