Triethylamine → HCID 58258314, 화합물

HRID 514590노트

반응식

HRID 514590 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 58258314HCID 58258314, 화합물수율 90%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6a8605a3396c4b34970f6139581df791
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107946B2

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