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Imidazole → HCID 59750865、化合物

HRID 748797
ノート
印刷プレビュー

反応式

HRID 748797 の反応式
[OH:1][CH2:2][CH2:3][N:4]([CH2:12][CH2:13][OH:14])[C:5](=[O:11])[O:6][C:7]([CH3:10])([CH3:9])[CH3:8].N1C=CN=C1.[C:20]([Si:24](Cl)([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)([CH3:23])([CH3:22])[CH3:21].CCCCCC>ClCCl.CN(C)C=O.C(OCC)(=O)C>[Si:24]([O:1][CH2:2][CH2:3][N:4]([CH2:12][CH2:13][OH:14])[C:5](=[O:11])[O:6][C:7]([CH3:8])([CH3:9])[CH3:10])([C:20]([CH3:23])([CH3:22])[CH3:21])([C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1
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 795ImidazoleHCID 8058HexaneHCID 94078tert-ButyldiphenylchlorosilaneHCID 4360601N-Boc-diethanolamine

生成物 1

HCID 59750865HCID 59750865、化合物収率 54%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒
HCID 22350042
dichloromethane N,N-dimethylformamide
溶媒

実験手順

In a dichloromethane/N,N-dimethylformamide (70 ml/70 ml) mixture were dissolved t-butyl N,N-bis(2-hydroxyethyl)carbamate (9.00 g, 43.8 mmol) and imidazole (2.60 g, 38.2 mmol), followed by the dropwise addition of t-butylchlorodiphenylsilane (8.1 ml, 31 mmol) at room temperature. After completion of the dropwise addition, the reaction mixture was stirred at room temperature for 14 hours. The residue obtained by concentrating the reaction mixture under reduced pressure was added with diethyl ether. The resulting mixture was washed with water and the organic layer was dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel chromatography, and the fraction obtained from the hexane:ethyl acetate=2:1 eluate was concentrated under reduced pressure, whereby the title compound (7.41 g, 16.7 mmol, 54%) was obtained as a colorless oil.

後処理

  1. additionAfter completion of the dropwise addition
  2. customThe residue obtained
  3. concentrationby concentrating the reaction mixture under reduced pressure
  4. additionwas added with diethyl ether
  5. washThe resulting mixture was washed with water
  6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  7. filtrationAfter filtration
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. customThe residue thus obtained

出典と根拠

ORDレコード
ord-5c5ca53811f642fea10bfd8baf26d2df
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07399775B2

反応ノート

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