Triethylamine → HCID 86589738, 화합물

HRID 2183688노트

반응식

HRID 2183688 반응식
Cl.Cl.[NH2:3][C@H:4]1[C:8]2([CH2:10][CH2:9]2)[CH2:7][NH:6][CH2:5]1.C(N(CC)CC)C.[F:18][B:19][F:20].[F:21][C:22]1[CH:23]=[C:24]2[C:29](=[C:30]([O:33][CH3:34])[C:31]=1F)[N:28]([C@@H:35]1[CH2:37][C@@H:36]1[F:38])[CH:27]=[C:26]([C:39]([OH:41])=[O:40])[C:25]2=[O:42]>CS(C)=O>[NH2:3][C@H:4]1[C:8]2([CH2:10][CH2:9]2)[CH2:7][N:6]([C:31]2[C:30]([O:33][CH3:34])=[C:29]3[C:24]([C:25](=[O:42])[C:26]([C:39]([OH:41])=[O:40])=[CH:27][N:28]3[C@@H:35]3[CH2:37][C@@H:36]3[F:38])=[CH:23][C:22]=2[F:21])[CH2:5]1.[F:18][B:19][F:20]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 23539486(7S)-5-Azaspiro[2.4]heptan-7-amine--hydrogen chloride (1/2)HCID 86589737HCID 86589737, 화합물

생성물 1

HCID 86589738HCID 86589738, 화합물수율 91%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

(7S)-7-Amino-5-azaspiro[2.4]heptane dihydrochloride (615 mg; 3.32 mmol) and triethylamine (1.40 ml) in dimethylsulfoxide (5 ml) was stirred for 20 minutes at room temperature. 6,7-Difluoro-1-[(1R, 2S)-2-fluoro-1-cyclopropyl]-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid difluoroboron chelate (1.00 g; 2.77 mmol) was added thereto, and the resultant mixture was stirred for 20 hours at room temperature. The reaction mixture was concentrated under reduced pressure, and purified water (50 ml) was added thereto. The pH of the resultant mixture was adjusted to 7.0 with aqueous 1N NaOH solution, and the aqueous layer of the mixture was taken up with chloroform (100 ml×5). The organic layer was dried over sodium sulfate, and the solvent was evaporated. The residue was purified through recrystallization from ethanol, to thereby yield 1.14 g of the title compound as pale yellow crystals (yield: 91%).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. custompurified water (50 ml)
  3. additionwas added
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. customthe solvent was evaporated
  6. customThe residue was purified through recrystallization from ethanol

출처 및 근거

ORD 기록
ord-ff2fbb58fdb54fef87387c976916a619
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900225B2

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