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Benzoyl chloride → HCID 18700007, 화합물

HRID 2288615
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HRID 2288615 반응식
[C:1]([Cl:9])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:10][C:11]1[O:15][C:14]([C:16]2[S:20][C:19]([CH2:21][N:22]3[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[CH:18][CH:17]=2)=[N:13][N:12]=1>N1C=CC=CC=1>[ClH:9].[N:22]1([CH2:21][C:19]2[S:20][C:16]([C:14]3[O:15][C:11]([NH:10][C:1](=[O:8])[C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)=[N:12][N:13]=3)=[CH:17][CH:18]=2)[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1
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참가 물질

4

반응물 2

HCID 7412Benzoyl chlorideHCID 18699937HCID 18699937, 화합물

생성물 1

HCID 18700007HCID 18700007, 화합물수율 57.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
80 °C

실험 절차

1.8 ml (15.0 mmol) of benzoyl chloride was added to 15 ml of pyridine solution containing 278 mg (1.0 mmol) of the compound of Example 43, and the mixture was stirred at 80° C. for 10 days. The reaction solution was concentrated under a reduced pressure, chloroform was added to the resulting residue, followed by washing with water and drying over anhydrous magnesium sulfate. The solvent was evaporated, the resulting residue was purified by a silica gel column chromatography. Then, the resulting crude crystals were recrystallized from ethanol-diisopropyl ether to give 241 mg of the title compound.

후처리

  1. concentrationThe reaction solution was concentrated under a reduced pressure, chloroform
  2. additionwas added to the resulting residue
  3. washby washing with water
  4. dry with materialdrying over anhydrous magnesium sulfate
  5. customThe solvent was evaporated
  6. customthe resulting residue was purified by a silica gel column chromatography
  7. customThen, the resulting crude crystals were recrystallized from ethanol-diisopropyl ether

출처 및 근거

ORD 기록
ord-d9986c1c58074a428f8f42c2e6dd893c
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06090804

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