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Ethylmorpholine → HCID 22732134, 화합물

HRID 1371537
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HRID 1371537 반응식
F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]=N1.[C:28]([O:32][C:33]([NH:35][CH:36]([CH2:40][C:41]1[CH:46]=[CH:45][C:44]([C:47]#[N:48])=[CH:43][CH:42]=1)[C:37]([OH:39])=O)=[O:34])([CH3:31])([CH3:30])[CH3:29].N1CCCC1.C(N1CCOCC1)C>CN(C=O)C>[C:28]([O:32][C:33]([NH:35][CH:36]([CH2:40][C:41]1[CH:46]=[CH:45][C:44]([C:47]#[N:48])=[CH:43][CH:42]=1)[C:37]([N:10]1[CH2:11][CH2:16][CH2:15][CH2:14]1)=[O:39])=[O:34])([CH3:29])([CH3:30])[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7525EthylmorpholineHCID 31268PyrrolidineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 43933462-Tert-butoxycarbonylamino-3-(4-cyano-phenyl)-propionic acid

생성물 1

HCID 22732134HCID 22732134, 화합물수율 79.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

7.5 g of BOP are added to a mixture of 4.06 g of 2-(tert-butoxycarbonylamino)-3-(4-cyanophenyl)propionic acid and 1.15 ml of pyrrolidine in 20 ml of DMF, and the mixture is stirred for 2 hours at RT, while maintaining the pH at 7 by adding N-ethylmorpholine. The reaction mixture is concentrated under vacuum and the residue is chromatographed on silica gel, eluting with a chloroform/MeOH mixture (95/5; v/v). 3.8 g of the expected product are obtained.

후처리

  1. temperaturewhile maintaining the pH at 7
  2. concentrationThe reaction mixture is concentrated under vacuum
  3. customthe residue is chromatographed on silica gel
  4. washeluting with a chloroform/MeOH mixture (95/5; v/v)

출처 및 근거

ORD 기록
ord-6518015e35704478a6f810ca1037f544
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157454B2

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