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Trifluoroacetic acid → 1-Methyl-3-(4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-2-yl)-urea

HRID 239104
ノート
印刷プレビュー

反応式

HRID 239104 の反応式
C(O)(C(F)(F)F)=O.C(OC([N:15]1[CH2:20][CH2:19][C:18]2[N:21]=[C:22]([NH:24][C:25]([NH:27][CH3:28])=[O:26])[S:23][C:17]=2[CH2:16]1)=O)(C)(C)C>C(Cl)(Cl)Cl>[CH3:28][NH:27][C:25]([NH:24][C:22]1[S:23][C:17]2[CH2:16][NH:15][CH2:20][CH2:19][C:18]=2[N:21]=1)=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 584408222-(3-Methyl-ureido)-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester

生成物 1

HCID 584407561-Methyl-3-(4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-2-yl)-urea収率 96%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

10% TFA in 60 ml chloroform was added to 2.3 g 2-(3-methyl-ureido)-6,7-dihydro-4H-thiazolo-[5,4-c]pyridine-5-carboxylic acid tert-butyl ester in 28 ml chloroform and stirred for 2 h at RT. The mixture was concentrated, the residue was diluted with chloroform and basified with 2.5 M aqueous potassium carbonate solution and extracted with chloroform. The organic layer was concentrated. The residue was washed with a mixture of 50% ethyl acetate and 50% hexane to yield 1.5 g of the desired product. (M+H)+: 213

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationThe mixture was concentrated
  2. additionthe residue was diluted with chloroform
  3. extractionextracted with chloroform
  4. concentrationThe organic layer was concentrated
  5. washThe residue was washed with a mixture of 50% ethyl acetate and 50% hexane

出典と根拠

ORDレコード
ord-d87b4939e96d4f208a0f06cf584b4876
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642774B2

反応ノート

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