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Chloroform → HCID 69100830, 화합물

HRID 394038
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HRID 394038 반응식
[CH2:1]([N:3]1[CH2:8][CH2:7][CH2:6][C@@H:5]([CH2:9][NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([C@@H:20]2[CH2:24][C@@H:23]([OH:25])[CH2:22][N:21]2[C:26](=[O:47])[CH2:27][C:28]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[O:19])=[O:12])[CH2:4]1)[CH3:2].[CH2:48](I)[CH3:49].C(Cl)(Cl)[Cl:52]>>[Cl-:52].[CH2:1]([N+:3]1([CH2:48][CH3:49])[CH2:8][CH2:7][CH2:6][C@@H:5]([CH2:9][NH:10][C:11]([C@H:13]2[CH2:17][CH2:16][CH2:15][N:14]2[C:18]([C@@H:20]2[CH2:24][C@@H:23]([OH:25])[CH2:22][N:21]2[C:26](=[O:47])[CH2:27][C:28]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)([C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)=[O:19])=[O:12])[CH2:4]1)[CH3:2]
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4

반응물 3

HCID 6212ChloroformHCID 6340IodoethaneHCID 69100640HCID 69100640, 화합물

생성물 1

HCID 69100830HCID 69100830, 화합물

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온도
70 °C

실험 절차

To 22 mg of (2R)-N-{((3S)-1-ethyl-3-piperidyl)methyl}-1-{(2S,4R)-4-hydroxy-1-(3,3,3-triphenylpropanoyl)pyrrolidin-2-yl}carbonylpyrrolidine-2-carboxamide, 1 ml of ethyl iodide was added at room temperature, followed by 2 hours' stirring at 70° C. The resultant reaction liquid was diluted with chloroform and the solvent was distilled off under reduced pressure. The resultant residue was dissolved in ultrapure water 0.6 ml/methanol 0.1 ml and the solution was developed on reversed phase medium-pressure liquid chromatograpy [ODS-AQ 120-S50 (YMC)]. Purification and anion exchange were conducted by pouring 20 ml of saturated brine, washing with 150 ml of ultrapure water and eluting the title compound with methanol/water=1/1, to provide 21 mg of the title compound as a white solid.

후처리

  1. customThe resultant reaction liquid
  2. distillationthe solvent was distilled off under reduced pressure
  3. dissolutionThe resultant residue was dissolved in ultrapure water 0.6 ml/methanol 0.1 ml
  4. customPurification and anion exchange
  5. additionby pouring 20 ml of saturated brine
  6. washwashing with 150 ml of ultrapure water
  7. washeluting the title compound with methanol/water=1/1

출처 및 근거

ORD 기록
ord-e54de950ac4f47c7a655ec69d97bb060
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06809108B1

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