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

HRID 1445333노트

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HRID 1445333 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6344Dichloromethane용매

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온도
22 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d35c19e78622421cba0f8b6e32e1d050
출처 데이터셋
uspto-grants-2010_02
특허 번호
US07666848B2

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