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2-Methyl-2-butene → HCID 90449616、化合物

HRID 1411294
ノート
印刷プレビュー

反応式

HRID 1411294 の反応式
[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([CH:17]=[O:18])[CH:15]=3)[N:10]([C:19]([NH:21][C:22]3[S:23][C:24]([Cl:27])=[CH:25][N:26]=3)=[O:20])[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2].CC(=CC)C.P([O-])(O)(O)=[O:34].[Na+].Cl([O-])=O.[Na+].[Cl-].[NH4+]>C(O)(C)(C)C.O>[C:1]([N:4]1[CH2:8][CH2:7][C:6]2([C:16]3[C:11](=[CH:12][CH:13]=[C:14]([C:17]([OH:34])=[O:18])[CH:15]=3)[N:10]([C:19](=[O:20])[NH:21][C:22]3[S:23][C:24]([Cl:27])=[CH:25][N:26]=3)[CH2:9]2)[CH2:5]1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 105532-Methyl-2-buteneHCID 25517Ammonium ChlorideHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphateHCID 90449869HCID 90449869、化合物

生成物 1

HCID 90449616HCID 90449616、化合物収率 87.2%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6386tert-Butanol溶媒

実験手順

1′-Acetyl-N-(5-chlorothiazol-2-yl)-5-formylspiro[indoline-3,3′-pyrrolidine]-1-carboxamide (7.6 mg, 0.0188 mmol) was dissolved in t-butanol (1.5 mL) and water (0.5 mL). Thereafter, 2-methyl-2-butene (52 μL, 0.50 mmol), sodium dihydrogen phosphate (14 mg, 0.113 mmol) and sodium chlorite (15 mg, 0.169 mmol) were added to the above obtained solution, and the thus obtained mixture was then stirred at room temperature for 3.3 hours. Thereafter, a saturated aqueous solution of ammonium chloride was added to the reaction solution, and the mixed solution was then extracted with chloroform:methanol=5:1. The organic layer was dried over anhydrous sodium sulfate, and was then concentrated in vacuo. The obtained residue was purified by silica gel column chromatography (chloroform:methanol=5:1) to obtain the captioned compound (6.9 mg, 87%) in the form of a white solid.

後処理

  1. extractionthe mixed solution was then extracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationwas then concentrated in vacuo
  4. customThe obtained residue was purified by silica gel column chromatography (chloroform:methanol=5:1)

出典と根拠

ORDレコード
ord-04ff4cfc3c0a4634b39675a77862a731
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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