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Ammonia → HCID 54308607, 화합물

HRID 231938
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HRID 231938 반응식
[CH:1]1([C:5]([NH:7][C@H:8]([C:24]([NH:26][CH:27]([P:35](=[O:40])([O:38]C)[O:36]C)[CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[O:25])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14]([O:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[O:15])=[O:6])[CH2:4][CH2:3][CH2:2]1.C[Si](Br)(C)C.C(O)(C)C.N>ClCCl.O>[CH:1]1([C:5]([NH:7][C@H:8]([C:24]([NH:26][CH:27]([P:35](=[O:36])([OH:40])[OH:38])[CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[O:25])[CH2:9][CH2:10][CH2:11][CH2:12][NH:13][C:14]([O:16][CH2:17][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)=[O:15])=[O:6])[CH2:4][CH2:3][CH2:2]1
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참가 물질

7

반응물 4

HCID 222AmmoniaHCID 3776IsopropanolHCID 76113BromotrimethylsilaneHCID 86743240HCID 86743240, 화합물

생성물 1

HCID 54308607HCID 54308607, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

The dimethyl ester product from part (e) (1.04 g., 1.81 mmole) is dissolved in dichloromethane (10 ml.) and treated with trimethysilylbromide (0.52 ml., 605 mg., 3.96 mmole). The mixture is stirred under argon overnight then concentrated in vacuo. Dioxane (15 ml.) and water (5 ml.) are added and the resulting mixture is stirred for 15 minutes and then concentrated. Residual water is chased three times with acetonitrile (20 ml.) giving 1.06 g. of [1-[[N2 -(cyclobutylcarbonyl)-N6 -[(phenylmethoxy)carbonyl]-L-lysyl]-2-phenylethyl]phosphonic acid as an organe-yellow foam. TLC (silica gel; isopropanol:ammonia:water, 7:2:1) Rf =0.42.

후처리

  1. concentrationthen concentrated in vacuo
  2. additionDioxane (15 ml.) and water (5 ml.) are added
  3. stirringthe resulting mixture is stirred for 15 minutes
  4. concentrationconcentrated
  5. customgiving 1.06 g

출처 및 근거

ORD 기록
ord-3043322370f843d3956b08799b3953b3
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04849414

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