Triphenylphosphine → 4-(5-Undecyl-pyrimidin-2-yl)phenyl (3-ethyl-cyclopentan-1-yl)methyl ether

HRID 1826556노트

반응식

HRID 1826556 반응식
N(C(OCC)=O)=NC(OCC)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:32]([C:43]1[CH:44]=[N:45][C:46]([C:49]2[CH:54]=[CH:53][C:52]([OH:55])=[CH:51][CH:50]=2)=[N:47][CH:48]=1)[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42].[CH2:56]([CH:58]1[CH2:62][CH2:61][CH:60]([CH2:63]O)[CH2:59]1)[CH3:57]>C1COCC1>[CH2:56]([CH:58]1[CH2:62][CH2:61][CH:60]([CH2:63][O:55][C:52]2[CH:51]=[CH:50][C:49]([C:46]3[N:47]=[CH:48][C:43]([CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[CH:44][N:45]=3)=[CH:54][CH:53]=2)[CH2:59]1)[CH3:57]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 22134208(3-Ethylcyclopentyl)methanolHCID 1356196824-(5-Undecylpyrimidin-2-yl)phenol

생성물 1

HCID 701128834-(5-Undecyl-pyrimidin-2-yl)phenyl (3-ethyl-cyclopentan-1-yl)methyl ether

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A fully reacted mixture of equimolar amounts of diethyl azodicarboxylate and triphenylphosphine in THF is admixed with equimolar amounts of 4-(5-undecyl-pyrimidin-2-yl)phenol and 3-ethyl-cyclopentan-1-yl-methanol (prepared by LiAlH4 reduction of methyl 3-ethyl-cyclopentanecarboxylic acid). The mixture is stirred for 24 h at room temperature and then evaporated to dryness under reduced pressure. Purification by chromatography (silica gel, dichloromethane) and recrystallization affords the target compound.

후처리

  1. customevaporated to dryness under reduced pressure
  2. customPurification
  3. customby chromatography (silica gel, dichloromethane) and recrystallization
  4. customaffords the target compound

출처 및 근거

ORD 기록
ord-b069b6d95c594dc887798e2bfe81c520
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07052742B1

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