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Iodine → HCID 59909851, 화합물

HRID 2183031
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인쇄 미리보기

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HRID 2183031 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.II.C(N(CC)CC)C.[CH:29]1([CH2:35][CH2:36][CH2:37][C@@H:38]([C:47]([NH:49][CH:50]([C:54]([O:56][CH3:57])=[O:55])[C:51](=[O:53])[CH3:52])=O)[CH2:39][C:40]([O:42][C:43]([CH3:46])([CH3:45])[CH3:44])=[O:41])[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1>O1CCCC1.O>[C:43]([O:42][C:40](=[O:41])[CH2:39][C@H:38]([C:47]1[O:53][C:51]([CH3:52])=[C:50]([C:54]([O:56][CH3:57])=[O:55])[N:49]=1)[CH2:37][CH2:36][CH2:35][CH:29]1[CH2:34][CH2:33][CH2:32][CH2:31][CH2:30]1)([CH3:44])([CH3:46])[CH3:45]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 807IodineHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 59909746HCID 59909746, 화합물

생성물 1

HCID 59909851HCID 59909851, 화합물수율 62.9%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

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온도
-78 °C

실험 절차

A suspension of triphenylphosphine (9.49 g, 36.18 mmol), iodine (7.98 g, 31.44 mmol) and triethylamine (8.49 ml, 60.75 mmol) in tetrahydrofuran was cooled to −78° C. then treated with tert-butyl (3R)-6-cyclohexyl-3-({[1-(methoxycarbonyl)-2-oxopropyl]amino}carbonyl)hexanoate (Preparation 68) (4.86 g, 11.80 mmol) over 15 minutes. The mixture was stirred at −78° C. for 30 minutes then at 0-5° C. for 2 hours. The mixture was diluted with water and extracted with dichloromethane. The combined organic layers were dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was purified by column chromatography on silica gel eluting with a gradient system of ethyl acetate:pentane (0:100 to 10:90) to afford the title compound as a colourless oil (2.92 g).

후처리

  1. waitat 0-5° C. for 2 hours
  2. extractionextracted with dichloromethane
  3. dry with materialThe combined organic layers were dried over anhydrous magnesium sulphate
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel eluting with a gradient system of ethyl acetate:pentane (0:100 to 10:90)

출처 및 근거

ORD 기록
ord-e3977aefc3104ac48d5042bc1b54308e
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06897306B2

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