Triethylamine → 3-Benzyloxy-5-isopropyl-N-methoxy-N-methylthiophene-2-carboxamide

HRID 1445333ノート

反応式

HRID 1445333 の反応式
[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([CH:14]([CH3:16])[CH3:15])[S:11][C:10]=1[C:17]([OH:19])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:21][NH:22][O:23][CH3:24].C(N(CC)CC)C>ClCCl.C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:13]=[C:12]([CH:14]([CH3:15])[CH3:16])[S:11][C:10]=1[C:17]([N:22]([O:23][CH3:24])[CH3:21])=[O:19])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 219612383-Benzyloxy-5-isopropyl-thiophene-2-carboxylic acid

生成物 1

HCID 219612223-Benzyloxy-5-isopropyl-N-methoxy-N-methylthiophene-2-carboxamide

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
22 °C

実験手順

860 mg of 3-benzyloxy-5-isopropyl-thiophene-2-carboxylic acid were dissolved in 30 ml of dichloromethane, and 560 mg of N,O-dimethylhydroxylamine hydrochloride and 2.3 of triethylamine were added. After 15 min at 22° C., 2.3 ml of a 50% strength 1-propanephosphonic anhydride solution in acetic acid were added, and the mixture was stirred at 22° C. for a further 18 h. The reaction mixture was washed twice with 20 ml of water each time and once with 70 ml of saturated sodium chloride solution. The organic phase was dried over sodium sulfate and concentrated.

後処理

  1. washThe reaction mixture was washed twice with 20 ml of water each time
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-d35c19e78622421cba0f8b6e32e1d050
出典データセット
uspto-grants-2010_02
特許番号
US07666848B2

反応ノート

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