Potassium Hydroxide → 1-(7-Acetylenyl-2-benzothiazolyl)-3-ethylurea

HRID 9121

반응식

HRID 9121 반응식
C[Si]([C:5]#[C:6][C:7]1[C:15]2[S:14][C:13]([NH:16][C:17]([NH:19][CH2:20][CH3:21])=[O:18])=[N:12][C:11]=2[CH:10]=[CH:9][CH:8]=1)(C)C.[OH-].[K+].CN(C=O)C.CO>CCCCCCC.CO>[C:6]([C:7]1[C:15]2[S:14][C:13]([NH:16][C:17]([NH:19][CH2:20][CH3:21])=[O:18])=[N:12][C:11]=2[CH:10]=[CH:9][CH:8]=1)#[CH:5]

참가 물질

6

반응물 3

HCID 14797Potassium HydroxideHCID 21901440N,N-dimethylformamide methanolHCID 219855381-(7-Trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea

생성물 1

HCID 219856501-(7-Acetylenyl-2-benzothiazolyl)-3-ethylurea수율 15.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8900Heptane용매

실험 절차

A mixture of 1-(7-trimethylsilylacetylenyl-2-benzothiazolyl)-3-ethylurea 2 (0.050 g, 0.16 mmol) and 1M aqueous KOH solution (0.16 mL, 0.16 mmol, 1.0 eq) in 1.5 mL of 2/1 mixture of DMF/MeOH was stirred at room temperature for about 2 hours. The mixture was taken up in 10 mL MeOH and the precipitation was filtered off. The mother liquid was concentrated and purified by prep HPLC to give the desired compound 0.006 g (15%). LC/MS 246 (M+1); LC retention time 2.77 min.

후처리

  1. customthe precipitation
  2. filtrationwas filtered off
  3. concentrationThe mother liquid was concentrated
  4. custompurified by prep HPLC

출처 및 근거

ORD 기록
ord-8abe128357e5495cb8583bed1bcfdda2
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091227B2

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