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Chloride → HCID 21201649, 화합물

HRID 1979380
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HRID 1979380 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6].Cl[C:14](Cl)([O:16]C(=O)OC(Cl)(Cl)Cl)Cl.[C:25]([C:29]([CH2:31][N:32]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=2[N:36]([C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=2[F:49])[CH2:35][CH:34]([NH2:50])[C:33]1=[O:51])=[O:30])([CH3:28])([CH3:27])[CH3:26].[Cl-]>O1CCCC1.C(N(CC)CC)C>[C:25]([C:29]([CH2:31][N:32]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=2[N:36]([C:43]2[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=2[F:49])[CH2:35][CH:34]([NH:50][C:14]([NH:1][C:2]2[CH:12]=[CH:11][CH:10]=[C:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH:3]=2)=[O:16])[C:33]1=[O:51])=[O:30])([CH3:28])([CH3:26])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 312ChlorideHCID 11400Ethyl 3-aminobenzoateHCID 94429TriphosgeneHCID 21201731HCID 21201731, 화합물

생성물 1

HCID 21201649HCID 21201649, 화합물수율 223.5%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회
HCID 8471Triethylamine용매

실험 절차

Ethyl 3-aminobenzoate (69 mg) was dissolved in tetrahydrofuran (10 ml), the solution was cooled on ice-water. Triphosgene (45 mg) was added at internal temperature 5° C., triethylamine (162 mg) was added thereto over 10 minutes period, the mixture was allowed to come to room temperature and stirred for 10 minutes. A solution of 1-tert-butylcarbonylmethyl-2-oxo-3-amino-5-(2-fluorophenyl)-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (150 mg) in tetrahydrofuran (5 ml), the mixture was additionally chloride. The organic layer was successively washed with water and saturated brine, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography(n-hexane:ethyl acetate=3:1), to thereby obtain 190 mg of the title compound as colorless crystals (Yield: 83%).

후처리

  1. temperaturethe solution was cooled on ice-water
  2. additionwas added
  3. customto come to room temperature
  4. washThe organic layer was successively washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography(n-hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-d58a158b89b14b26afd1e6ec05a8f33c
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06239131B1

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