Hydrochloric Acid → 1-(6-Acetylenyl-2-benzothiazolyl)-3-ethylurea

HRID 9131

反応式

HRID 9131 の反応式
C[Si]([C:5]#[C:6][C:7]1[CH:21]=[CH:20][C:10]2[N:11]=[C:12]([NH:14][C:15]([NH:17][CH2:18][CH3:19])=[O:16])[S:13][C:9]=2[CH:8]=1)(C)C.[OH-].[K+].Cl>CO.CCOC(C)=O>[C:6]([C:7]1[CH:21]=[CH:20][C:10]2[N:11]=[C:12]([NH:14][C:15]([NH:17][CH2:18][CH3:19])=[O:16])[S:13][C:9]=2[CH:8]=1)#[CH:5]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 219855421-(6-Trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea

生成物 1

HCID 219855921-(6-Acetylenyl-2-benzothiazolyl)-3-ethylurea収率 5.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1-(6-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea (0.0710 g, 0.22 mmol) and 1M aqueous KOH solution (1.22 mL, 1.22 mmol, 5.5 eq) in 1.5 mL MeOH was stirred at room temperature for about 2 hours. The mixture acidified with 1 M HCl, then taken up in 20 mL AcOEt, and the aqueous phase was extracted with 10 mL AcOEt. The combined organic portions were dried (MgSO4), concentrated, and purified by HPLC to give the desired compound 0.003 g (5%). LC/MS 246 (M+1); LC retention time 2.84 min.

後処理

  1. extractionthe aqueous phase was extracted with 10 mL AcOEt
  2. dry with materialThe combined organic portions were dried (MgSO4)
  3. concentrationconcentrated
  4. custompurified by HPLC

出典と根拠

ORDレコード
ord-e28f5a27454f477e9bdcf8a67a519fdf
出典データセット
uspto-grants-2006_08
特許番号
US07091227B2

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