Sodium Chloride → HCID 12090302、化合物

HRID 427250

反応式

HRID 427250 の反応式
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].C(N(CC)CC)C.Cl[C:19]([O:21][CH3:22])=[O:20].[Cl-].[Na+]>C(Cl)(Cl)Cl>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:19](=[O:20])[O:21][CH3:22]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 27249803-Bromobenzylamine hydrochloride

生成物 1

HCID 12090302HCID 12090302、化合物収率 87%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a suspension of 10.0 g of 3-bromobenzylamine hydrochloride in chloroform (100 ml), 9.55 g of triethylamine was added at room temperature. To this solution, 4.67 g of methyl chloroformate was dropwise added under cooling with ice, followed by stirring at room temperature for 2 hours. The reaction solution was poured into a sodium chloride aqueous solution, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals.

後処理

  1. additionwas added at room temperature
  2. temperatureunder cooling with ice
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-2e7b3b0e1e124827b5f8cf77d7fe0b6a
出典データセット
uspto-grants-2001_11
特許番号
US06313071B1

関連ノート

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