Bromoacetic Acid → HCID 22220859、化合物

HRID 1794043ノート

反応式

HRID 1794043 の反応式
[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

反応物 3

HCID 6227Bromoacetic AcidHCID 6342AcetonitrileHCID 99892951-(1,3-Thiazol-2-yl)ethan-1-ol

生成物 1

HCID 22220859HCID 22220859、化合物収率 33.1%

試薬・触媒・溶媒 1

HCID 21959252Acetonitrile methanol溶媒

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

  1. waitstored at 4 C for 17 hr
  2. customThe crystals which separated
  3. filtrationwere filtered out
  4. customrecrystalized from methanol/acetonitrile/ether

出典と根拠

ORDレコード
ord-3578d31f7a1c40e7a0a8a59f0a6e75f9
出典データセット
uspto-grants-2006_04
特許番号
US07022721B1

反応ノート

読み込み中…