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HCID 68636737, 화합물 → HCID 25125758, 화합물

HRID 1929789
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HRID 1929789 반응식
[Si]([O:8][CH2:9][C:10](=[CH2:42])[C:11]([N:13]1[CH2:18][CH2:17][CH:16]([O:19][C:20]2[CH:21]=[C:22]3[C:27](=[CH:28][C:29]=2[O:30][CH3:31])[N:26]=[CH:25][N:24]=[C:23]3[NH:32][C:33]2[CH:38]=[CH:37][C:36]([Cl:39])=[C:35]([Cl:40])[C:34]=2[F:41])[CH2:15][CH2:14]1)=[O:12])(C(C)(C)C)(C)C>O1CCCC1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:40][C:35]1[C:34]([F:41])=[C:33]([NH:32][C:23]2[C:22]3[C:27](=[CH:28][C:29]([O:30][CH3:31])=[C:20]([O:19][CH:16]4[CH2:17][CH2:18][N:13]([C:11](=[O:12])[C:10]([CH2:9][OH:8])=[CH2:42])[CH2:14][CH2:15]4)[CH:21]=3)[N:26]=[CH:25][N:24]=2)[CH:38]=[CH:37][C:36]=1[Cl:39]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 68636737HCID 68636737, 화합물

생성물 1

HCID 25125758HCID 25125758, 화합물수율 51%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 2724141Tetrabutylammonium Fluoride용매

실험 절차

140 mg of the compound obtained in step 3) was diluted with 3 ml of tetrahydrofuran, and 1.1 ml of a 1.0M tetra-n-butyl ammonium fluoride-containing tetrahydrofuran solution was added thereto. The resulting mixture was incubated at room temperature for three hours. After the reaction terminated, a saturated sodium hydrogen carbonate was added, and the resulting solution was extracted twice with chloroform. The organic layer was dried over anhydrous sodium sulfate, filtered and distilled under a reduced pressure. The resulting residue was purified by column chromatography (ethyl acetate:methylene chloride:methanol=7:7:1) to obtain the title compound (58 mg, 51%).

후처리

  1. additionwas added
  2. customAfter the reaction terminated
  3. additiona saturated sodium hydrogen carbonate was added
  4. extractionthe resulting solution was extracted twice with chloroform
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. distillationdistilled under a reduced pressure
  8. customThe resulting residue was purified by column chromatography (ethyl acetate:methylene chloride:methanol=7:7:1)

출처 및 근거

ORD 기록
ord-75473993af0e4eee876a2fb768ffb83e
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08188102B2

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