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Phenol → 1-Acetyl-6-bromo-5-[(1,2,3,5,6,8a-hexahydroindolizin-7-yl)methoxy]indoline

HRID 1274236
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HRID 1274236 반응식
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([OH:14])=[C:10]([Br:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[CH2:15]1[CH:23]2[N:18]([CH2:19][CH2:20][C:21]([CH2:24]O)=[CH:22]2)[CH2:17][CH2:16]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O.C1(O)C=CC=CC=1>C1COCC1.C(OCC)(=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:14][CH2:24][C:21]3[CH2:20][CH2:19][N:18]4[CH:23]([CH:22]=3)[CH2:15][CH2:16][CH2:17]4)=[C:10]([Br:13])[CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
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참가 물질

8

반응물 5

HCID 996PhenolHCID 11776Triphenylphosphine2회HCID 220568ethyl N-ethoxycarbonyliminocarbamate2회HCID 219483801-(6-Bromo-5-hydroxy-2,3-dihydro-1H-indol-1-yl)ethan-1-oneHCID 221209331,2,3,5,6,8a-Hexahydroindolizine-7-methanol

생성물 1

HCID 22120926
1-Acetyl-6-bromo-5-[(1,2,3,5,6,8a-hexahydroindolizin-7-yl)methoxy]indoline
수율 13.3%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

1-Acetyl-6-bromo-5-hydroxyindoline (Tetrahedron, 1973, 29(8), 1115) (1.24 g, 4.8 mmol), 1,2,3,5,6,8a-hexahydroindolizine-7-methanol (D2, 0.74 g, 4.8 mmol) and triphenylphosphine (1.27 g, 4.8 mmol) were stirred under Ar in dry THF (50 ml) as diethyl azodicarboxylate (0.76 ml, 4.8 mmol) was added dropwise. The mixture was stirred for 1 h, diluted with ethyl acetate, and extracted with dil. HCl. The extract was basified with potassium carbonate, and extracted with chloroform. This extract was dried (Na2SO4) and evaporated to give a dark oil. Further treatment of this oil as above with the phenol, triphenylphosphine and diethyl azodicarboxylate caused reaction to proceed further. Chromatography on silica, eluting with 0-20% methanol/dichloromethane, gave the title compound (0.25 g, 13%) as a brown gum.

후처리

  1. additionwas added dropwise
  2. extractionextracted with dil. HCl
  3. extractionextracted with chloroform
  4. dry with materialThis extract was dried (Na2SO4)
  5. customevaporated
  6. customto give a dark oil
  7. customreaction
  8. washChromatography on silica, eluting with 0-20% methanol/dichloromethane

출처 및 근거

ORD 기록
ord-72d97894ddc44ef3a5690cf2bd344327
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06156783

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