Methanol → 1-(6-(3-Aminopropanoyl)-2-benzothiazolyl)-3-ethylurea

HRID 9138

反応式

HRID 9138 の反応式
[C:1]([CH2:3][C:4]([C:6]1[CH:20]=[CH:19][C:9]2[N:10]=[C:11]([NH:13][C:14]([NH:16][CH2:17][CH3:18])=[O:15])[S:12][C:8]=2[CH:7]=1)=[O:5])#[N:2].CO>[Pt](=O)=O.C(Cl)(Cl)Cl>[NH2:2][CH2:1][CH2:3][C:4]([C:6]1[CH:20]=[CH:19][C:9]2[N:10]=[C:11]([NH:13][C:14]([NH:16][CH2:17][CH3:18])=[O:15])[S:12][C:8]=2[CH:7]=1)=[O:5]

参加物

5

反応物 2

HCID 887MethanolHCID 219855541-(6-(2-Cyanoacetyl)-2-benzothiazolyl)-3-ethylurea

生成物 1

HCID 219855561-(6-(3-Aminopropanoyl)-2-benzothiazolyl)-3-ethylurea収率 121.5%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 6212Chloroform溶媒

実験手順

A suspension of 1-(6-(2-cyanoacetyl)-2-benzothiazolyl)-3-ethylurea (0.56 g, 1.94 mmol) and platinum (IV) oxide (0.176 g, 0.78 mmol, 0.40 eq) in 50 mL of 2/3 mixture of MeOH and chloroform was purged and bubbled with hydrogen gas. It was stirred under hydrogen gas for about 2 days. The mixture was filtered and concentrated to give 0.689 g (quantitative yield) desired compound. LC/MS 292.9 (M+1); LC retention time 1.80 min. HPLC purification gave corresponding acetic acid salt. LC/MS 292.9 (M+1); LC retention time 1.80 min. In a similar reaction, compound as an acetate salt form was obtained after HPLC purification.

後処理

  1. customwas purged
  2. custombubbled with hydrogen gas
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-ec7552d657b74d9cb90ee4e75ae57522
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

関連ノート

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