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Isopropyl chloroformate → Isopropyl 3,5-difluoro-phenylcarbamate

HRID 1179478
ノート
印刷プレビュー

反応式

HRID 1179478 の反応式
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[F:11][C:12]1[CH:13]=[C:14]([CH:16]=[C:17]([F:19])[CH:18]=1)[NH2:15].Cl[C:21]([O:23][CH:24]([CH3:26])[CH3:25])=[O:22]>C1COCC1.CCOCC>[F:11][C:12]1[CH:13]=[C:14]([NH:15][C:21](=[O:22])[O:23][CH:24]([CH3:26])[CH3:25])[CH:16]=[C:17]([F:19])[CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7917Isopropyl chloroformateHCID 965953,5-DifluoroanilineHCID 2733832Lithium hexamethyldisilazane

生成物 1

HCID 58978077Isopropyl 3,5-difluoro-phenylcarbamate

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium bis(trimethylsilyl) amide (1.0 M solution in tetrahydrofuran, 542 mL, 0.542 mol) was added to a solution of 3,5-difluoroaniline (35 g, 0.271 mol) in THF (60 mL) at 0° C. Isopropyl chloroformate (1M solution in toluene, 406 mL, 0.406 mol) was then added dropwise at 0° C. and the mixture allowed to warm to room temperature over 2 h. The reaction mixture was diluted with ether and washed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine and dried (MgSO4). Solvent was removed under vacuum and the residue was triturated in hexanes to obtain the title compound.

後処理

  1. washwashed with 1N hydrochloric acid, water, saturated aqueous sodium bicarbonate, brine
  2. dry with materialdried (MgSO4)
  3. customSolvent was removed under vacuum
  4. customthe residue was triturated in hexanes

出典と根拠

ORDレコード
ord-e00ebf9ef67c46d2949943269d0d0ab3
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07279494B2

反応ノート

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