Bromoacetic Acid → HCID 22220859、化合物
反応式
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH:6]([OH:8])[CH3:7].[Br:9][CH2:10][C:11](O)=[O:12].C(#N)C>C(#N)C.CO>[Br-:9].[CH3:7][CH:6]1[C:2]2[S:1][CH:5]=[CH:4][N+:3]=2[CH2:10][C:11](=[O:12])[O:8]1参加物
5
実験手順
1-(2-Thiazolyl)ethanol (0.5 g, 3.87 mmole), bromoacetic acid (0.537 g, 3.86 mmole), and acetonitrile (0.125 mL) were heated in an oil bath with stirring at 105 C. for 6 hr. The mixture was dissolved in 5 mL 4:1 acetonitrile/methanol and stored at 4 C. for 17 hr. The crystals which separated were filtered out and combined from two identical runs, and recrystalized from methanol/acetonitrile/ether to give a total of 0.32 g of the title compound, mp 214-215.5 C. Calcd for C7H8NO2SBr: C 33.5; H 3.20; N 5.59; found: C 33.62; H 3.16; N 5.61.
後処理
- waitfor 17 hr
- customThe crystals which separated
- filtrationwere filtered out
- customrecrystalized from methanol/acetonitrile/ether
出典と根拠
- ORDレコード
- ord-876c05a7c0c04c07ab773ebccf6a47fe
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06777557B2
反応ノート
読み込み中…