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Acetic Anhydride → HCID 71245377, 화합물

HRID 1186017
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HRID 1186017 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C:12]1([CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:16](=[O:26])[NH:17][C@@H:18]([C@H:23]([OH:25])[CH3:24])[C:19]([O:21][CH3:22])=[O:20])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CCN(CC)CC.[CH3:41][C:42](OC(C)=O)=[O:43]>C1COCC1.C(Cl)Cl>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][C:12]1([C:16](=[O:26])[NH:17][C@@H:18]([C@H:23]([O:25][C:42](=[O:43])[CH3:41])[CH3:24])[C:19]([O:21][CH3:22])=[O:20])[CH2:27][C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 71245383HCID 71245383, 화합물

생성물 1

HCID 71245377HCID 71245377, 화합물수율 76.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

Compound 4 (3 g, 6.60 mmol) was dissolved in THF (30 mL), Et3N (1.11 mL, 7.92 mmol) and Ac2O (742 mg, 7.26 mmol) were added at RT. The reaction mixture was stirred at RT for 2 h. The volatiles were evaporated under reduced pressure and the residue obtained was diluted with CH2Cl2 and washed with dilute HCl. The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The crude residue was purified by column chromatography using 30% EtOAc/Hexane as eluent to yield compound 5 (2.5 g, 76%).

후처리

  1. customThe volatiles were evaporated under reduced pressure
  2. customthe residue obtained
  3. washwashed with dilute HCl
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-bf5ebc82e0664112a529b0b23a89ccf5
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08673843B2

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