Triethylamine → HCID 58258314、化合物

HRID 514590ノート

反応式

HRID 514590 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8]Cl)=[CH:4][C:3]=1[Cl:10].[CH3:11][CH2:12][N:13](CC)[CH2:14][CH3:15].N1CCCC1>C1COCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:13]2[CH2:14][CH2:15][CH2:11][CH2:12]2)=[CH:4][C:3]=1[Cl:10]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31268PyrrolidineHCID 233343071-Bromo-2-chloro-4-(chloromethyl)benzene

生成物 1

HCID 58258314HCID 58258314、化合物収率 90%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-bromo-2-chloro-4-(chloromethyl)-benzene (25.2 g, 105.03 mmol) and Et3N (16.1 ml, 115.53 mmol) in THF (150 ml) was stirred at r.t. Pyrrolidine (8.2 g, 115.53 mmol) was added dropwise. The r.m. was stirred overnight at r.t. and was then concentrated in vacuo. The residue was taken up into water and extracted with CH2Cl2 (3×100 ml). The combined organic layer was washed with saturated NaHCO3 and brine, and was then dried (MgSO4), filtered and the solvent was evaporated in vacuo. Yield: 25.8 g of 1-[(4-bromo-3-chlorophenyl)methyl]-pyrrolidine (90% yield, crude product; used in next reaction step, without further purification).

後処理

  1. concentrationwas then concentrated in vacuo
  2. extractionextracted with CH2Cl2 (3×100 ml)
  3. washThe combined organic layer was washed with saturated NaHCO3 and brine
  4. dry with materialwas then dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-6a8605a3396c4b34970f6139581df791
出典データセット
uspto-grants-2015_08
特許番号
US09107946B2

反応ノート

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