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

HRID 9131

반응식

HRID 9131 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e28f5a27454f477e9bdcf8a67a519fdf
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

연결된 노트

불러오는 중…