Ethyl cyanoacetate → HCID 19616892、化合物

HRID 31061ノート

反応式

HRID 31061 の反応式
C[O-].[Na+].[CH3:4][O:5][CH2:6][CH2:7][CH2:8][NH:9][C:10]([NH2:12])=[S:11].[C:13]([CH2:15][C:16](OCC)=[O:17])#[N:14]>C(O)C>[NH2:14][C:13]1[N:9]([CH2:8][CH2:7][CH2:6][O:5][CH3:4])[C:10](=[S:11])[NH:12][C:16](=[O:17])[CH:15]=1

参加物

5

反応物 3

HCID 7764Ethyl cyanoacetateHCID 27740941-(3-Methoxypropyl)-2-thioureaHCID 10942334Sodium Methoxide

生成物 1

HCID 19616892HCID 19616892、化合物収率 48.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Sodium methoxide (0.81 g, 21.2 mmol, 1.05 eq.) was added to a solution of 3-methoxypropylthiourea (3.00 g, 20.2 mmol) in ethanol (10 mL). Ethyl cyanoacetate (2.18 mL, 20.2 mmol) in ethanol (10 mL) was added and the resulting white slurry was heated to reflux for 2.5 h. The solvent was evaporated and the remaining pale brown oil was treated with 2M acetic acid (15 mL,). The white crystals were filtered off and washed with acetic acid to give the title compound (2.10 g, 48%).

後処理

  1. temperaturethe resulting white slurry was heated
  2. temperatureto reflux for 2.5 h
  3. customThe solvent was evaporated
  4. additionthe remaining pale brown oil was treated with 2M acetic acid (15 mL,)
  5. filtrationThe white crystals were filtered off
  6. washwashed with acetic acid

出典と根拠

ORDレコード
ord-cc6dcb2bbcda45e6942cf4787f9a8a66
出典データセット
uspto-grants-2008_09
特許番号
US07425560B2

反応ノート

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