Acetic Anhydride → 2-thiocyanatoethyl acetate

HRID 2078636ノート

反応式

HRID 2078636 の反応式
[S-:1][C:2]#[N:3].[C:4]([O:7][C:8](=O)[CH3:9])(=[O:6])[CH3:5]>N1C=CC=CC=1.ClCCl>[C:4]([O:7][CH2:8][CH2:9][S:1][C:2]#[N:3])(=[O:6])[CH3:5]

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 9322Thiocyanate

生成物 1

HCID 2327002-thiocyanatoethyl acetate

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 2-bromoethanol (7.0 g) and potassium thiocyanate (5.4 g) in methanol (40 ml) was refluxed for 7 hours. After precipitate was filtered off, the filtrate was evaporated under reduced pressure. The residue was suspended in chloroform/methanol (5/1). The precipitate was filtered off. The filtrate was evaporated under reduced pressure to give the thiocyanate (4.4 g). To a mixture of the thiocyanate in pyridine (4.8 ml)/dichloromethane (20 ml) was added acetic anhydride (5.3 ml) in dichloromethane (5 ml) at 5° C. The mixture was stirred at room temperature for 6 hours. The precipitate was filtered off. The filtrate was washed with water, dried over sodium sulfate and evaporated under reduced pressure to give 2-thiocyanatoethyl acetate (5.6 g).

後処理

  1. filtrationThe precipitate was filtered off
  2. washThe filtrate was washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-f271f7cbb72c49e5987e2aedb10e3a54
出典データセット
uspto-grants-2011_04
特許番号
US07928264B2

反応ノート

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