Triethylamine → HCID 178521527, 화합물

HRID 606449노트

반응식

HRID 606449 반응식
[NH:1]1[CH:5]=[N:4][C:3]([SH:6])=[N:2]1.I[CH2:8][CH2:9][OH:10].C(N(CC)CC)C>C(O)C>[NH:1]1[CH:5]=[N:4][C:3]([S:6][CH2:8][CH2:9][OH:10])=[N:2]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12225IodoethanolHCID 178527894HCID 178527894, 화합물

생성물 1

HCID 178521527HCID 178521527, 화합물수율 35%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 1H-1,2,4-triazole-3-thiol (14.7 g, 145 mmol), 2-iodoethanol (25.0 g, 145 mmol) and triethylamine (14.7 g, 145 mmol) in ethanol (400 mL) was stirred at 80° C. for 15 hr. The reaction mixture was concentrated under reduced pressure, and the residue was acidified with water and 1N hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over sodium sulfate, and concentrated. The obtained oil was purified by silica gel column chromatography (10%-100% ethyl acetate/hexane) to give the title compound as a colorless oil (7.30 g, 35%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe obtained oil was purified by silica gel column chromatography (10%-100% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-062d5293625f490eb1a0a19b3947a226
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915267B2

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