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Triphenylphosphine → (s)-2-Amino-n-(1-carbamoyl-4-guanidino-butyl)-5-[2-(2,4-dichlorophenyl)ethoxy]benzamide

HRID 433036
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HRID 433036 반응식
[NH2:1][C@H:2]([C:24]([OH:26])=O)[CH2:3][CH2:4][CH2:5][NH:6][C:7](=[NH:23])[N:8](C(OC(C)(C)C)=O)C(OC(C)(C)C)=O.[OH:27][C:28]1[CH:29]=[CH:30][C:31]([N+:37]([O-])=O)=[C:32]([CH:36]=1)[C:33]([OH:35])=O.CC(C)[N:42]=C=NC(C)C.C1C=CC2N(O)N=NC=2C=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:78][C:79]1[CH:84]=[C:83]([Cl:85])[CH:82]=[CH:81][C:80]=1[CH2:86][CH2:87]O.CC(OC(/N=N/C(OC(C)C)=O)=O)C>CN(C=O)C.C1COCC1>[NH2:37][C:31]1[CH:30]=[CH:29][C:28]([O:27][CH2:87][CH2:86][C:80]2[CH:81]=[CH:82][C:83]([Cl:85])=[CH:84][C:79]=2[Cl:78])=[CH:36][C:32]=1[C:33]([NH:1][C@H:2]([C:24](=[O:26])[NH2:42])[CH2:3][CH2:4][CH2:5][NH:6][C:7]([NH2:8])=[NH:23])=[O:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 7

HCID 11776TriphenylphosphineHCID 118825-Hydroxy-2-nitrobenzoic acidHCID 12734DiisopropylcarbodiimideHCID 757711-HydroxybenzotriazoleHCID 27340992,4-Dichlorophenethyl alcoholHCID 5363146Diisopropyl azodicarboxylateHCID 178454311HCID 178454311, 화합물

생성물 1

HCID 178512851(s)-2-Amino-n-(1-carbamoyl-4-guanidino-butyl)-5-[2-(2,4-dichlorophenyl)ethoxy]benzamide

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

Rink resin (306 mg; loading 0.43 mmol/g) functionalized with Arg(Boc)2 was coupled with 146 mg of 5-hydroxy-2-nitrobenzoic acid in the presence of DIC (136 mg) and HOBt (140 mg) in DMF (2 ml) for 3 h at room temperature. The resin was then washed and treated with a 15% solution of benzyltrimethylammonium hydroxide in DMF for 60 min. The resin was washed with DMF, 10% acetic acid in DMF, DMF and DCM and dried in vacuo for 4 h. The dried resin was washed with anhydrous THF and mixed with 534 mg (2 mmol) of triphenylphosphane, 422 mg (2 mmol) of 2-(2,4-dichlorophenyl)ethanol and 400 μl (2 mmol) of DIAD in dry THF. The mixture was kept overnight at room temperature. The resin was washed and treated with 415 mg of tin dichloride monohydrate in 2 ml of DMF and 0.5 ml of trifluoroethanol. The reduction was continued overnight at room temperature. The resin was washed and dried, and the final product was cleaved off and processed as described in Example 1.

후처리

  1. washThe resin was then washed
  2. additiontreated with a 15% solution of benzyltrimethylammonium hydroxide in DMF for 60 min
  3. washThe resin was washed with DMF, 10% acetic acid in DMF, DMF and DCM
  4. customdried in vacuo for 4 h
  5. washThe dried resin was washed with anhydrous THF
  6. washThe resin was washed
  7. additiontreated with 415 mg of tin dichloride monohydrate in 2 ml of DMF and 0.5 ml of trifluoroethanol
  8. waitThe reduction was continued overnight at room temperature
  9. washThe resin was washed
  10. customdried

출처 및 근거

ORD 기록
ord-5f2d0b808a76495195fdc7ec8cb0a7f9
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06664393B2

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