Iodine → Tert-butyl[2-(5-isopropyl-[1,3,4]oxadiazol-2-yl)-ethyl]-carbamate

HRID 2110934노트

반응식

HRID 2110934 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.II.C(N(CC)CC)C.[C:29]([O:33][C:34](=[O:47])[NH:35][CH2:36][CH2:37][C:38]([NH:40][NH:41][C:42](=[O:46])[CH:43]([CH3:45])[CH3:44])=O)([CH3:32])([CH3:31])[CH3:30]>ClCCl>[C:29]([O:33][C:34](=[O:47])[NH:35][CH2:36][CH2:37][C:38]1[O:46][C:42]([CH:43]([CH3:45])[CH3:44])=[N:41][N:40]=1)([CH3:32])([CH3:31])[CH3:30]

참가 물질

6

반응물 4

HCID 807IodineHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 57637099tert-butyl [3-(N'-isobutyryl-hydrazino)-3-oxo-propyl]-carbamate

생성물 1

HCID 57637115Tert-butyl[2-(5-isopropyl-[1,3,4]oxadiazol-2-yl)-ethyl]-carbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

20.00 g (43.00 mmol) PS-triphenylphosphine are placed in 240 ml dichloromethane, 10.88 g (42.87 mmol) iodine are added. The mixture is stirred for 0.1 hours at ambient temperature, then 12.10 ml (87.29 mmol) triethylamine are added dropwise. 5.83 g (21.33 mmol) tert-butyl[3-(N′-isobutyryl-hydrazino)-3-oxo-propyl]-carbamate dissolved in 150 ml dichloromethane are added. The reaction mixture is stirred for 24 hours at ambient temperature, then the precipitate is filtered off. The filtrate is evaporated down and purified by chromatography.

후처리

  1. additionare added
  2. stirringThe reaction mixture is stirred for 24 hours at ambient temperature
  3. filtrationthe precipitate is filtered off
  4. customThe filtrate is evaporated down
  5. custompurified by chromatography

출처 및 근거

ORD 기록
ord-997cd74062a5482f852208c962d0eb51
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517995B2

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