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Oxalyl chloride → HCID 53752128, 화합물

HRID 1602489
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HRID 1602489 반응식
C(Cl)(=O)C(Cl)=O.[S:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH:16]=[CH:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=1.Cl.[NH2:28][C:29]1[CH:34]=[C:33]([CH2:35][CH2:36][CH2:37][S:38]([C:41]2[CH:46]=[CH:45][C:44]([Cl:47])=[CH:43][CH:42]=2)(=[O:40])=[O:39])[CH:32]=[CH:31][C:30]=1[OH:48]>CN(C)C=O.ClCCl.N1C=CC=CC=1>[S:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH:16]=[CH:17][C:18]1[CH:19]=[CH:20][C:21]([C:22]([NH:28][C:29]2[CH:34]=[C:33]([CH2:35][CH2:36][CH2:37][S:38]([C:41]3[CH:46]=[CH:45][C:44]([Cl:47])=[CH:43][CH:42]=3)(=[O:40])=[O:39])[CH:32]=[CH:31][C:30]=2[OH:48])=[O:24])=[CH:25][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 65578Oxalyl chlorideHCID 52170324-[2-(2-Benzothiazolyl)vinyl]benzoic acidHCID 196115102-Amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride

생성물 1

HCID 53752128HCID 53752128, 화합물수율 65%

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매
HCID 1049
Pyridine
용매
HCID 6344Dichloromethane용매2회

실험 절차

At -78° C., oxalyl chloride (135 mg, 1.06 mmol) was added to a mixture of 4-[2-(2-benzothiazolyl)vinyl]benzoic acid (247 mg, 0.88 mmol), dimethylformamide (one drop) and dichloromethane (10 ml), and the resulting mixture was stirred at room temperature for 2 hours and then concentrated under reduced pressure. Under ice-cooling, the resulting compound was gradually added to a mixture of 2-amino-4-[3-(4-chlorophenylsulfonyl)propyl]phenol hydrochloride (320 mg, 0.88 mmol), pyridine (3 ml) and dichloromethane (10 ml), and the resulting mixture was stirred at room temperature for 12 hours. The reaction solution was concentrated under reduced pressure, water was added to the resulting residue, and the mixture was heated until reflux and then cooled. Then, the solid material formed was collected by filtration and dried under reduced pressure. Ethanol (10 ml) was added to the resulting solid material, and the mixture was heated until reflux and then cooled. The crystals formed were collected by filtration and dried under reduced pressure to give 4-[2-(2-benzothiazolyl)vinyl]-5'-[3-(4-chlorophenylsulfonyl)propyl]-2'-hydroxybenzanilide (335 mg, 0.57 mmol, 65%) as colorless crystals.

후처리

  1. concentrationconcentrated under reduced pressure
  2. temperatureUnder ice-cooling
  3. stirringthe resulting mixture was stirred at room temperature for 12 hours
  4. concentrationThe reaction solution was concentrated under reduced pressure, water
  5. additionwas added to the resulting residue
  6. temperaturethe mixture was heated
  7. temperatureuntil reflux
  8. temperaturecooled
  9. customThen, the solid material formed
  10. filtrationwas collected by filtration
  11. customdried under reduced pressure
  12. additionEthanol (10 ml) was added to the resulting solid material
  13. temperaturethe mixture was heated
  14. temperatureuntil reflux
  15. temperaturecooled
  16. customThe crystals formed
  17. filtrationwere collected by filtration
  18. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-153fffa770894a1fb0b2a21f4fbf59b0
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05981559

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