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Water → HCID 54339944, 화합물

HRID 745621
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HRID 745621 반응식
CC(C)([O-])C.[K+].COP([CH2:13][C:14]([O:16][CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[O:15])(OC)=O.[CH3:24][NH:25][C:26](=[O:46])[C@H:27]([CH2:37][C:38]1[CH:43]=[CH:42][C:41]([O:44][CH3:45])=[CH:40][CH:39]=1)[NH:28][C:29](=[O:36])[C:30](=O)[CH2:31][CH:32]([CH3:34])[CH3:33].O>CN(C)C=O>[CH3:24][NH:25][C:26](=[O:46])[C@H:27]([CH2:37][C:38]1[CH:39]=[CH:40][C:41]([O:44][CH3:45])=[CH:42][CH:43]=1)[NH:28][C:29](=[O:36])[C:30]([CH2:31][CH:32]([CH3:33])[CH3:34])=[CH:13][C:14]([O:16][CH2:17][C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 2773759Benzyl DimethylphosphonoacetateHCID 14303083N-(4-Methyl-2-oxopentanoyl)-O-methyl-L-tyrosine N-MethylamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 54339944HCID 54339944, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

Potassium tertiary butoxide (2.1 g., 0.0188 mol.) was suspended in dry dimethylformamide (50 mls.). To the suspension was added benzyl dimethylphosphonoethanoate (4.6 g., 0.0187 mol.) at room temperature. The reaction mixture was stirred at room temperature for 0.5 hours. N-(4-Methyl-2-oxopentanoyl)-O-methyl-L-tyrosine N-Methylamide (3.0 g., 0.00913 mol) was added portionwise to the reaction mixture over a period of 10 minutes to yield a red solution. The red solution was stirred at room temperature for 4 hours, and then poured into water (500 mls.). The resulting mixture obtained was extracted with ethyl acetate (2×100 mls.) and the ethyl acetate extract was washed with water (2×25 mls.), brine (25 mls.) and dried over anhydrous magnesium sulfate. The ethyl acetate was removed by evaporation in vacuo to yield a crude solid product (4.2 g.). The crude product was purified by recrystallization from a mixture of ethyl acetate and hexane to yield E and Z N-[3-(benzyloxycarbonyl)-2-(2-methylpropyl)propenoyl]-O-methyl-L-tyrosine N-methylamide as a light brown crystalline solid. (m.p. 167°-9° C. Found: C, 68.3; H, 7.1; N, 6.3 %. C25H30N2O5 requires C, 68.5; H, 6.9; N, 6.4%).

후처리

  1. customto yield a red solution
  2. stirringThe red solution was stirred at room temperature for 4 hours
  3. customThe resulting mixture obtained
  4. extractionwas extracted with ethyl acetate (2×100 mls.)
  5. extractionthe ethyl acetate extract
  6. washwas washed with water (2×25 mls.), brine (25 mls.)
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe ethyl acetate was removed by evaporation in vacuo
  9. customto yield a crude solid product (4.2 g.)
  10. customThe crude product was purified by recrystallization from a mixture of ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-b505a2b4fed242cda9e58937f8bf82ca
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04599361

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