Hydrochloric Acid → H-Gly-Leu-Ala-OBzl HCl

HRID 4984

반응식

HRID 4984 반응식
[NH:1](C(OC(C)(C)C)=O)[CH2:2][C:3]([NH:5][C@H:6]([C:11]([NH:13][C@H:14]([C:16]([O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[O:17])[CH3:15])=[O:12])[CH2:7][CH:8]([CH3:10])[CH3:9])=[O:4].FC(F)(F)C(O)=O.N[C@H](C(N[C@H](C(OCC1C=CC=CC=1)=O)C)=O)CC(C)C.FC(F)(F)C([O-])=O.[ClH:68]>CCOCC.C(OCC)(=O)C>[NH2:1][CH2:2][C:3]([NH:5][C@H:6]([C:11]([NH:13][C@H:14]([C:16]([O:18][CH2:19][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)=[O:17])[CH3:15])=[O:12])[CH2:7][CH:8]([CH3:10])[CH3:9])=[O:4].[ClH:68]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 6422Trifluoroacetic acidHCID 84468TrifluoroacetateHCID 16742166H-Leu-Ala-OBzlHCID 131717744Boc-Gly-Leu-Ala-OBzl

생성물 1

HCID 131718105H-Gly-Leu-Ala-OBzl HCl

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매

실험 절차

Boc-Gly-Leu-Ala-OBzl was prepared by coupling Boc-Gly-OH (5.70 g, 32.6 mmoles) to H-Leu-Ala-OBzl using the mixed anhydride procedure described in Example 2. The product (13.8 g) was obtained as an amorphous solid. Boc-Gly-Leu-Ala-OBzl was deblocked with trifluoroacetic acid by the procedure described for the preparation of H-Leu-Ala-OBzl except that the trifluoroacetate salt was soluble in ether. The preparation was dissolved in ethyl acetate and treated with anhydrous hydrogen chloride. The resulting product was precipitated by the addition of ether to yield 7.7 g of H-Gly-Leu-Ala-OBzl HCl in a first crop.

후처리

  1. customThe resulting product was precipitated by the addition of ether

출처 및 근거

ORD 기록
ord-1e9e6ea312024abbb5827b12a87dd34a
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242904

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