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Hydrochloric Acid → HCID 131709984, 화합물

HRID 1580881
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HRID 1580881 반응식
[NH:1](C(OCC1C=CC=CC=1)=O)[C@H:2]([C:11]([NH:13][C@H:14]([C:22]([O:24][CH3:25])=[O:23])[CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:12])[CH2:3][C:4](=[O:10])[O:5][C:6]([CH3:9])([CH3:8])[CH3:7].Cl.[H][H]>CO.O1CCOCC1.[Pd]>[NH2:1][C@H:2]([C:11]([NH:13][C@H:14]([C:22]([O:24][CH3:25])=[O:23])[CH2:15][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)=[O:12])[CH2:3][C:4](=[O:10])[O:5][C:6]([CH3:7])([CH3:8])[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 11340682HCID 11340682, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 131709984HCID 131709984, 화합물수율 110.1%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 887Methanol용매
HCID 31275
1,4-Dioxane
용매

실험 절차

48.6 g of Z-Asp(OtBu)-Phe-OCH3 in 700 ml of methanol are decarbobenzoxylated in a duck-shaped flask at room temperature after adding 33.5 ml of 3 N hydrogen chloride in dioxane and 5 g of 10 % strength palladium catalyst on charcoal. After the hydrogen uptake has ended the mixture is filtered and the filtrate evaporated. 38.7 g of a white foam are obtained. In a thin layer chromatogram on silica gel in chloroformmethanol (9:1) Rf = 0.60; in chloroform-acetone (1:1) Rf = 0.58; Rf102E =0.42. The product is employed for the subsequent condensation without additonal purification.

후처리

  1. filtrationis filtered
  2. customthe filtrate evaporated

출처 및 근거

ORD 기록
ord-30a53d436ec64018a41d12f7feca4e25
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03934008

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