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Triphenylphosphine → HCID 66877137, 화합물

HRID 1863977
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HRID 1863977 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:20]([O:27][C:28]([N:30]1[CH2:35][C@H:34]([O:36][CH2:37][C:38]2[CH:39]=[CH:40][C:41]3[O:46][CH2:45][CH2:44][N:43]([CH2:47][CH2:48][CH2:49][O:50][CH3:51])[C:42]=3[CH:52]=2)[C@@H:33]([C:53]2[CH:58]=[CH:57][C:56]([CH2:59][O:60][CH2:61][C@@H:62]([CH3:66])[CH2:63][O:64][CH3:65])=[CH:55][CH:54]=2)[C@H:32]([CH2:67][N:68]=[N+]=[N-])[CH2:31]1)=[O:29])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>CO.O1CCCC1.O.N>[CH2:20]([O:27][C:28]([N:30]1[CH2:35][C@H:34]([O:36][CH2:37][C:38]2[CH:39]=[CH:40][C:41]3[O:46][CH2:45][CH2:44][N:43]([CH2:47][CH2:48][CH2:49][O:50][CH3:51])[C:42]=3[CH:52]=2)[C@@H:33]([C:53]2[CH:58]=[CH:57][C:56]([CH2:59][O:60][CH2:61][C@@H:62]([CH3:66])[CH2:63][O:64][CH3:65])=[CH:55][CH:54]=2)[C@H:32]([CH2:67][NH2:68])[CH2:31]1)=[O:29])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 2

HCID 11776TriphenylphosphineHCID 86629099HCID 86629099, 화합물

생성물 1

HCID 66877137HCID 66877137, 화합물

시약·촉매·용매 4

HCID 222Ammonia용매HCID 887Methanol용매HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

7.128 mmol of triphenylphosphine are added to a solution of 5.940 mmol of (3S,4R,5R)-3-azidomethyl-4-[4-((S)-3-methoxy-2-methyl-propoxymethyl)-phenyl]-5-[4-(3-methoxy-propyl)-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethoxy]-piperidine-1-carboxylic acid benzyl ester in 20 ml of methanol, 20 ml of tetrahydrofuran, 5 ml of water and 3.56 ml of concentrated aqueous ammonia (25%) at room temperature. After overnight stirring, the reaction mixture is partitioned between tert-butyl methyl ether and 5:1 water/saturated aqueous sodium bicarbonate solution. The aqueous layer is extracted with tert-butyl methyl ether—the combined organic layers are washed successively with water and brine, dried with sodium sulfate and evaporated. The residue is purified by flash chromatography (SiO2 60F) to afford the title compound as a yellow oil. Rf=0.42 (dichloromethane-methanol-25% ammonia conc. 200:20:1); Rt=4.64 (gradient I).

후처리

  1. customthe reaction mixture is partitioned between tert-butyl methyl ether and 5:1 water/saturated aqueous sodium bicarbonate solution
  2. extractionThe aqueous layer is extracted with tert-butyl methyl ether—the combined organic layers
  3. washare washed successively with water and brine
  4. dry with materialdried with sodium sulfate
  5. customevaporated
  6. customThe residue is purified by flash chromatography (SiO2 60F)

출처 및 근거

ORD 기록
ord-949a414a1d9549018559b49ecdf62e7a
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07625893B2

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