Diisopropyl Ether → HCID 178455965, 화합물

HRID 1982308노트

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HRID 1982308 반응식
[NH:1]([C:17]([O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[O:18])[C@H:2]([C:7]([O:9]N1C(=O)CCC1=O)=O)[C@H:3]([CH2:5][CH3:6])[CH3:4].CCN(CC)CC.C(OC(C)C)(C)C.[NH2:41][C@H:42]([C:49]([NH:51][C@H:52]([C:65]([O:67][CH3:68])=[O:66])[CH2:53][CH2:54][CH2:55][CH2:56][NH:57][C:58]([O:60][C:61]([CH3:64])([CH3:63])[CH3:62])=[O:59])=[O:50])[CH2:43][C:44]1[N:48]=[CH:47][NH:46][CH:45]=1>CN(C=O)C>[NH:1]([C:17]([O:19][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)=[O:18])[C@H:2]([C:7]([NH:41][C@H:42]([C:49]([NH:51][C@H:52]([C:65]([O:67][CH3:68])=[O:66])[CH2:53][CH2:54][CH2:55][CH2:56][NH:57][C:58]([O:60][C:61]([CH3:64])([CH3:63])[CH3:62])=[O:59])=[O:50])[CH2:43][C:44]1[N:48]=[CH:47][NH:46][CH:45]=1)=[O:9])[C@H:3]([CH2:5][CH3:6])[CH3:4]

참가 물질

6

반응물 4

HCID 7914Diisopropyl EtherHCID 8471TriethylamineHCID 13361528Z-Ile-OSuHCID 178501448H-His-Lys(Boc)-OMe

생성물 1

HCID 178455965HCID 178455965, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.32 g of Z-Ile-OSu [G. W. Anderson et. al., J. Amer. Chem. Soc. 86, 1839 (1964)] are dissolved in the above solution of H-His-Lys(Boc)-OMe in approximately 10 ml of DMF and mixed with 0.41 ml of NEt3. The whole is left to stand for 8 hours at room temperature, 15 ml of diisopropyl ether are added, and the whole is homogenised and filtered. The residue obtained by filtering with suction is dissolved in 15 ml of methanol and added at 0° to 23 ml of aqueous NaHCO3 solution. The resulting precipitate is filtered off, washed with H2O, dried and dissolved and reprecipitated from MeOH/ethyl acetate/petroleum ether, yielding Z-Ile-His-Lys(Boc)-OMe in the form of amorphous powder; Rf (B)=0.65; Rf (I)=0.48.

후처리

  1. waitThe whole is left
  2. filtrationfiltered
  3. customThe residue obtained
  4. filtrationby filtering with suction
  5. dissolutionis dissolved in 15 ml of methanol
  6. additionadded at 0° to 23 ml of aqueous NaHCO3 solution
  7. filtrationThe resulting precipitate is filtered off
  8. washwashed with H2O
  9. customdried
  10. dissolutiondissolved
  11. customreprecipitated from MeOH/ethyl acetate/petroleum ether

출처 및 근거

ORD 기록
ord-ce8789a81b9d458eb11bf86f4f86ebac
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595677

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