Triethylamine → tert-Butyl 3-bromobenzylcarbamate

HRID 390622ノート

反応式

HRID 390622 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:11](OC([O-])=O)([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12].C(N(CC)CC)C>ClCCl>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:11](=[O:12])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27249803-Bromobenzylamine hydrochlorideHCID 22064466Tert-butyldicarbonate

生成物 1

HCID 11033439tert-Butyl 3-bromobenzylcarbamate収率 102.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 25 g (110 mmol) of 3-bromobenzylamine hydrochloride and 24.5 g (110 mmol) of tert-butyl dicarbonate in 250 mL of dichloromethane in the presence of 15.6 mL (110 mmol) of triethylamine is stirred at room temperature for 16 hours. The reaction medium is washed with water, the phases are separated by settling and the organic phase is dried over sodium sulfate. The solvent is evaporated off and 32.4 g (100%) of tert-butyl (3-bromobenzyl)carbamate are obtained in the form of crystals.

後処理

  1. washThe reaction medium is washed with water
  2. customthe phases are separated
  3. dry with materialthe organic phase is dried over sodium sulfate
  4. customThe solvent is evaporated off

出典と根拠

ORDレコード
ord-e4f9b643759e42af80358c77fd71f19e
出典データセット
uspto-grants-2013_02
特許番号
US08383652B2

反応ノート

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