Sodium Iodide → 2'-Isobutyl-4-methylvalerohydrazide

HRID 1386568노트

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HRID 1386568 반응식
ClCCCS([N:8]([CH2:37][CH:38]([CH3:40])[CH3:39])[NH:9][C:10](=[O:36])[C@@H:11]([C@@H](C(=O)NOC1CCCCO1)C/C=C/C1C=CC=CC=1)[CH2:12][CH:13]([CH3:15])[CH3:14])(=O)=O.[I-].[Na+].C(NCC)C>C(C(C)=O)C.C(OCC)(=O)C>[CH2:37]([NH:8][NH:9][C:10](=[O:36])[CH2:11][CH2:12][CH:13]([CH3:15])[CH3:14])[CH:38]([CH3:40])[CH3:39]

참가 물질

6

반응물 3

HCID 5238Sodium IodideHCID 8021DiethylamineHCID 86757192(E)-2'-(3-chloropropylsulphonyl)-2(R)-[1(S)-[(tetrahydro-2(RS)-pyranyloxy)carbamoyl]-4-phenyl-3-butenyl]-2'-isobutyl-4-methylvalerohydrazide

생성물 1

HCID 179023992'-Isobutyl-4-methylvalerohydrazide

시약·촉매·용매 2

HCID 6569Methyl Ethyl Ketone용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

A solution of 0.60 g of (E)-2′-(3-chloropropylsulphonyl)-2(R)-[1(S)-[(tetrahydro-2(RS)-pyranyloxy)carbamoyl]-4-phenyl-3-butenyl]-2′-isobutyl-4-methylvalerohydrazide in 10 ml of methyl ethyl ketone was treated with 0.18 g of sodium iodide and 1.04 ml of diethylamine. The mixture was heated at 80° C. for 4 hours and then at 60° C. for 48 hours. The mixture was diluted with ethyl acetate, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulphate and evaporated. The residue was purified by column chromatography on silica gel using methanol/dichloromethane (1:9) for the elution to give 0.16 g of (E)-2′-[3-(diethylamino)propylsulphonyl]-2(R) -[1(S)-(tetrahydro-2(RS)-pyranyloxy)carbamoyl]-4-phenyl-3-butenyl]-2′-isobutyl-4-methylvalerohydrazide in the form of a gum.

후처리

  1. washwashed with water and saturated aqueous sodium chloride
  2. dry with materialdried over anhydrous magnesium sulphate
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washfor the elution

출처 및 근거

ORD 기록
ord-aa5eec3e35e3463bbf7efb9f8ee4d054
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265446B1

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