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

HRID 2110934ノート

反応式

HRID 2110934 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-997cd74062a5482f852208c962d0eb51
出典データセット
uspto-grants-2009_04
特許番号
US07517995B2

反応ノート

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