Ethyl 3-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-2-carboxylate → HCID 178508937、化合物

HRID 215745

反応式

HRID 215745 の反応式
C([O:3][C:4]([C:6]1[S:10][C:9]2[CH2:11][CH2:12][CH2:13][CH2:14][C:8]=2[C:7]=1[NH2:15])=O)C.Cl.Cl[C:18]([NH2:20])=[NH:19]>COCCOCCOC>[NH2:20][C:18]1[NH:15][C:7]2[C:8]3[CH2:14][CH2:13][CH2:12][CH2:11][C:9]=3[S:10][C:6]=2[C:4](=[O:3])[N:19]=1

参加物

4

反応物 2

HCID 312340Ethyl 3-amino-4,5,6,7-tetrahydrobenzo[b]thiophene-2-carboxylateHCID 3084509Chloroformamidinium chloride

生成物 1

HCID 178508937HCID 178508937、化合物収率 95.5%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

反応条件

温度
160 °C

実験手順

A 48 mL sealed tube was charged with 3-amino-4,5,6,7-tetrahydro-benzo[b]thiophene-2-carboxylic acid ethyl ester (2.8 g, 12.3 mmol), chloroformamidine hydrochloride (2.0 g, 17.2 mmol), and diethylene glycol dimethyl ether (24.6 mL). The tube was sealed and heated to 160° C. for 12 h with vigorous stirring. Filtration afforded the desired compound as a beige solid (2.6 g). MS: No signal. 1H NMR (400 MHz, d6-DMSO) δ ppm 2.84-2.73 (m, 2H), 2.58-2.51 (m, 2H), 1.89-1.70 (m, 4H).

後処理

  1. customA 48 mL sealed tube
  2. customThe tube was sealed
  3. filtrationFiltration

出典と根拠

ORDレコード
ord-f0a4c69cac35436a9c47ea9285d5f640
出典データセット
uspto-grants-2012_06
特許番号
US08193178B2

関連ノート

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