Triethylamine → Ethyl 2-(3,3-dimethylbutyrylamino)-4,5,6,7-tetrahydrobenzthiazol-4-carboxylate

HRID 1394104

반응식

HRID 1394104 반응식
Br.[NH2:2][C:3]1[S:4][C:5]2[CH2:11][CH2:10][CH2:9][CH:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:6]=2[N:7]=1.C(N(CC)CC)C.[C:24]([CH2:28][C:29](Cl)=[O:30])([CH3:27])([CH3:26])[CH3:25]>C(#N)C>[CH3:25][C:24]([CH3:27])([CH3:26])[CH2:28][C:29]([NH:2][C:3]1[S:4][C:5]2[CH2:11][CH2:10][CH2:9][CH:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:6]=2[N:7]=1)=[O:30]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 815143,3-Dimethylbutanoyl chlorideHCID 87730500Ethyl 2-amino-4,5,6,7-tetrahydrobenzthiazole-4-carboxyate hydrobromide

생성물 1

HCID 59681875Ethyl 2-(3,3-dimethylbutyrylamino)-4,5,6,7-tetrahydrobenzthiazol-4-carboxylate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
0 °C

실험 절차

To a solution of ethyl 2-amino-4,5,6,7-tetrahydrobenzthiazole-4-carboxyate hydrobromide (0.92 g, 0.3 mol) in acetonitrile (25 mL) there was added triethylamine (Et3N, 0.41 g, 0.4 mol). Following cooling to 0° C., tert-butylacetyl chloride (0.55 g, 0.4 mol) was slowly added, and the resultant mixture was then stirred overnight at room temperature. Following removal of the solvent and purification by column chromatography, there was obtained ethyl 2-(3,3-dimethylbutyrylamino)-4,5,6,7-tetrahydrobenzthiazol-4-carboxylate in a yield of 185 mg (corresponding to 19% of theory).

후처리

  1. customremoval of the solvent and purification by column chromatography

출처 및 근거

ORD 기록
ord-318e770d7ce649978a8738cfab6f72d1
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07348347B2

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