Dichloromethane → (E)-3-(7-oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)acrylic Acid Hydrochloride

HRID 83005노트

반응식

HRID 83005 반응식
[OH-].[Na+].CN1CC[C:7]2([CH2:18][C:17]3[C:12](=[N:13][CH:14]=[C:15](/[CH:19]=[CH:20]/[C:21]([O:23]CC)=[O:22])[CH:16]=3)[NH:11][C:10]2=[O:26])CC1.[Cl:27]CCl>C(O)C>[ClH:27].[O:26]=[C:10]1[NH:11][C:12]2[N:13]=[CH:14][C:15](/[CH:19]=[CH:20]/[C:21]([OH:23])=[O:22])=[CH:16][C:17]=2[CH2:18][CH2:7]1

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 68338070HCID 68338070, 화합물

생성물 1

HCID 66905305(E)-3-(7-oxo-5,6,7,8-tetrahydro-1,8-naphthyridin-3-yl)acrylic Acid Hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
45 °C

실험 절차

An aqueous solution of sodium hydroxide (1N, 7.83 mL) was added to a solution of (E)-ethyl 3-(1′-methyl-2-oxo-2,4-dihydro-1H-spiro[[1,8]naphthyridine-3,4′-piperidine]-6-yl)acrylate (860 mg, 2.61 mmol) in a mixture of dichloromethane (10 mL) and ethanol (10 mL) at room temperature. The reaction mixture was stirred at 45° C. overnight then concentrated to dryness. The residue was acidified by addition of an aqueous solution of hydrochloric acid (1N, 30 mL) until pH 1. The resulting solid was filtered and washed with water and diethyl ether. The title product was obtained as a white solid (586 mg, 66%).

후처리

  1. concentrationthen concentrated to dryness
  2. additionThe residue was acidified by addition of an aqueous solution of hydrochloric acid (1N, 30 mL) until pH 1
  3. filtrationThe resulting solid was filtered
  4. washwashed with water and diethyl ether

출처 및 근거

ORD 기록
ord-85f5005b038c4cd78e18e59ada939277
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846711B2

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