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

HRID 9121

反応式

HRID 9121 の反応式
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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8900Heptane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-8abe128357e5495cb8583bed1bcfdda2
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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