Methylamine → 2-(3-Methyl-ureido)-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester

HRID 239103ノート

反応式

HRID 239103 の反応式
[CH3:1][NH2:2].[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][C:13]2[N:16]=[C:17]([NH:19][C:20]([O:22]C3C=CC=CC=3)=O)[S:18][C:12]=2[CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4]>CN(C=O)C.O>[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][C:13]2[N:16]=[C:17]([NH:19][C:20]([NH:2][CH3:1])=[O:22])[S:18][C:12]=2[CH2:11]1)=[O:9])([CH3:4])([CH3:5])[CH3:6]

参加物

5

反応物 2

HCID 6329MethylamineHCID 866860322-Phenoxycarbonylamino-6,7-dihydro-4H-thiazolo(5,4-c)pyridine-5-carboxylic acid tert-butyl ester

生成物 1

HCID 584408222-(3-Methyl-ureido)-6,7-dihydro-4H-thiazolo[5,4-c]pyridine-5-carboxylic acid tert-butyl ester収率 90.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

25 mg methylamine was added to 200 mg 2-phenoxycarbonylamino-6,7-dihydro-4H-thiazolo-[5,4-c]pyridine-5-carboxylic acid tert-butyl ester in 25 mL DMF. The reaction was stirred for 12 h at RT, diluted with water and extracted with ethyl acetate. The organic layer was washed with brine solution and concentrated. The residue was purified by column chromatographie (silica gel, eluent: 40% ethylacetate in hexane) to give 151 mg of desired product. (M+H)+: 313

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine solution
  3. concentrationconcentrated
  4. customThe residue was purified by column chromatographie (silica gel, eluent: 40% ethylacetate in hexane)

出典と根拠

ORDレコード
ord-2185d9e6a0074cbcbc33185c38921d33
出典データセット
uspto-grants-2014_02
特許番号
US08642774B2

反応ノート

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