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Ammonium Chloride → HCID 90449861、化合物

HRID 1411303
ノート
印刷プレビュー

反応式

HRID 1411303 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:10]3([CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11]3)[CH2:9][N:8]([C:22]([O:24][CH2:25][CH2:26][Si:27]([CH3:30])([CH3:29])[CH3:28])=[O:23])[C:5]2=[CH:6][CH:7]=1.COC1C=CC=C(OC)C=1C1C=CC=CC=1P(C1CCCCC1)C1CCCCC1.[Br-].[CH2:61]([O:63][C:64](=[O:69])[CH2:65][CH2:66][CH2:67][Zn+])[CH3:62].[Cl-].[NH4+]>O1CCCC1.C([O-])(=O)C.C([O-])(=O)C.[Pd+2]>[CH2:61]([O:63][C:64](=[O:69])[CH2:65][CH2:66][CH2:67][C:2]1[CH:3]=[C:4]2[C:10]3([CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:19])[CH3:20])=[O:16])[CH2:11]3)[CH2:9][N:8]([C:22]([O:24][CH2:25][CH2:26][Si:27]([CH3:30])([CH3:29])[CH3:28])=[O:23])[C:5]2=[CH:6][CH:7]=1)[CH3:62]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenylHCID 90449581HCID 90449581、化合物HCID 178471550HCID 178471550、化合物

生成物 1

HCID 90449861HCID 90449861、化合物収率 70%

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 8028Tetrahydrofuran溶媒

実験手順

The 1-(2-(trimethylsilyl)ethyl) 1′-tert-butyl 5-bromospiro[indoline-3,3′-pyrrolidine]-1,1′-dicarboxylate (100 mg, 0.201 mmol) obtained in Step 2 of Example 383 was dissolved in tetrahydrofuran (1.5 mL). Thereafter, palladium diacetate (10.0 mg, 0.045 mmol), S-Phos (33.0 mg, 0.080 mmol), and 4-ethoxy-4-oxobutylzinc bromide (0.5 M tetrahydrofuran solution, 0.5 mL) were added to the above obtained solution at room temperature, and the thus obtained mixture was then stirred at room temperature for 14 hours. Thereafter, a saturated aqueous solution of ammonium chloride was added to the reaction solution, and the mixed solution was then extracted with chloroform. The organic layer was washed with brine, and was then dried over anhydrous sodium sulfate, followed by concentration in vacuo. The obtained residue was purified by silica gel column chromatography (hexane ethyl acetate=10:1) to obtain 1-(2-(trimethylsilyl)ethyl) 1′-tert-butyl 5-(4-ethoxy-4-oxobutyl)spiro[indoline-3,3′-pyrrolidine]-1,1′-dicarboxylate (75.2 mg, 70%.) in the form of a white solid.

後処理

  1. extractionthe mixed solution was then extracted with chloroform
  2. washThe organic layer was washed with brine
  3. dry with materialwas then dried over anhydrous sodium sulfate
  4. concentrationfollowed by concentration in vacuo
  5. customThe obtained residue was purified by silica gel column chromatography (hexane ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-07532465253d4cb1b5a5ff8072295bb6
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921576B2

反応ノート

読み込み中…

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