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Nitromethane → tert-Butyl [1-(2-chlorophenyl)-2-nitroethyl]carbamate

HRID 220658
ノート
印刷プレビュー

反応式

HRID 220658 の反応式
[N+:1]([CH3:4])([O-:3])=[O:2].C(N(CC)C(C)C)(C)C.[Cl:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1/[CH:21]=[N:22]/[C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26]>>[Cl:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[CH:21]([NH:22][C:23](=[O:29])[O:24][C:25]([CH3:27])([CH3:26])[CH3:28])[CH2:4][N+:1]([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6375NitromethaneHCID 81531DiisopropylethylamineHCID 12195069tert-butyl (NE)-N-[(2-chlorophenyl)methylidene]carbamate

生成物 1

HCID 59536890tert-Butyl [1-(2-chlorophenyl)-2-nitroethyl]carbamate

実験手順

A quantity of 16 ml (295.41 mmol) of nitromethane was admixed with 436 μl (2.50 mmol) of N,N-diisopropylethylamine and the yellow solution was stirred at RT for 1 h. Then 2.0 g (8.34 mmol) of the compound from Example 111A were added and the mixture was stirred overnight at RT. All of the volatile constituents were removed on a rotary evaporator. The residue was dissolved in 9 ml of isopropanol in the heat of boiling, and the solution was then cooled to 0° C. The white solid precipitated was filtered off with suction and washed with a little cold isopropanol. Drying in an HV gave 1.18 g (47% of theory) of the title compound.

後処理

  1. stirringthe mixture was stirred overnight at RT
  2. customAll of the volatile constituents were removed on a rotary evaporator
  3. dissolutionThe residue was dissolved in 9 ml of isopropanol in the
  4. temperatureheat
  5. temperaturethe solution was then cooled to 0° C
  6. customThe white solid precipitated
  7. filtrationwas filtered off with suction
  8. washwashed with a little cold isopropanol
  9. customDrying in an HV

出典と根拠

ORDレコード
ord-1bd025acb08c4ea3ae72e9c00a9a91f3
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08202895B2

反応ノート

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