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Borohydride → HCID 58828971, 화합물

HRID 1171450
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HRID 1171450 반응식
[BH4-].[CH2:2]([C:9]1[N:10]([CH3:15])[C:11]([SH:14])=[N:12][N:13]=1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].I[C:17]1[CH:36]=[CH:35][C:20]([CH2:21][NH:22][C:23]2[CH:28]=[CH:27][C:26]([CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[CH:25][CH:24]=2)=[C:19]([O:37][CH2:38][CH2:39][CH3:40])[CH:18]=1>O1CCCC1.C(O)C>[CH2:33]([O:32][C:30](=[O:31])[CH2:29][C:26]1[CH:27]=[CH:28][C:23]([NH:22][CH2:21][C:20]2[CH:35]=[CH:36][C:17]([S:14][C:11]3[N:10]([CH3:15])[C:9]([CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])=[N:13][N:12]=3)=[CH:18][C:19]=2[O:37][CH2:38][CH2:39][CH3:40])=[CH:24][CH:25]=1)[CH3:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 28123BorohydrideHCID 58828974HCID 58828974, 화합물HCID 178442555HCID 178442555, 화합물

생성물 1

HCID 58828971HCID 58828971, 화합물

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매2회

실험 절차

2.647 g (6.62 mmol, 3 eq) of resin-supported borohydride and 30 mg (0.06 mmol, 0.03 eq) of bis(bipyridine)dibromonickel (II) are added to a solution of 0.706 g (3.31 mmol, 1.5 eq) of 5-heptyl-4-methyl-4H-[1,2,4]-triazole-3-thiol in 10 ml of tetrahydrofuran/ethanol 5/5. To the suspension obtained there is added a solution of 100 mg (0.22 mmol, 1 eq) of ethyl [4-(4-iodo-2-propoxybenzylamino)phenyl]acetate in 10 ml of tetrahydrofuran/ethanol 5/5. The reaction mixture is stirred overnight under reflux. After returning to room temperature, the reaction medium is filtered, concentrated and then chromatographed on silica gel (heptane/ethyl acetate 40/60). After evaporation of the solvents, 0.750 g (63%) of the expected compound is recovered.

후처리

  1. customTo the suspension obtained there
  2. temperatureunder reflux
  3. customAfter returning to room temperature
  4. filtrationthe reaction medium is filtered
  5. concentrationconcentrated
  6. customchromatographed on silica gel (heptane/ethyl acetate 40/60)
  7. customAfter evaporation of the solvents, 0.750 g (63%) of the expected compound
  8. customis recovered

출처 및 근거

ORD 기록
ord-451756e1e3eb4ffaa47f27b4a5a7d69c
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07829588B2

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