Triethylamine → HCID 178521527、化合物

HRID 606449ノート

反応式

HRID 606449 の反応式
[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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 12225IodoethanolHCID 178527894HCID 178527894、化合物

生成物 1

HCID 178521527HCID 178521527、化合物収率 35%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-062d5293625f490eb1a0a19b3947a226
出典データセット
uspto-grants-2011_03
特許番号
US07915267B2

反応ノート

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