Triphenylphosphine → 2-[4-[(5E)-5-Decen-1-yloxy]phenyl]-5-[(5,5,6,6,7,7,8,8,8-nonafluorooctyl)oxy]pyrimidine

HRID 1882750노트

반응식

HRID 1882750 반응식
CCOC(/N=N/C(OCC)=O)=O.[F:13][C:14]([F:43])([C:33]([F:42])([F:41])[C:34]([F:40])([F:39])[C:35]([F:38])([F:37])[F:36])[CH2:15][CH2:16][CH2:17][CH2:18][O:19][C:20]1[CH:21]=[N:22][C:23]([C:26]2[CH:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=2)=[N:24][CH:25]=1.[CH2:44](O)[CH2:45][CH2:46][CH2:47]/[CH:48]=[CH:49]/[CH2:50][CH2:51][CH2:52][CH3:53].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH2:44]([O:32][C:29]1[CH:28]=[CH:27][C:26]([C:23]2[N:22]=[CH:21][C:20]([O:19][CH2:18][CH2:17][CH2:16][CH2:15][C:14]([F:13])([F:43])[C:33]([F:41])([F:42])[C:34]([F:39])([F:40])[C:35]([F:36])([F:37])[F:38])=[CH:25][N:24]=2)=[CH:31][CH:30]=1)[CH2:45][CH2:46][CH2:47]/[CH:48]=[CH:49]/[CH2:50][CH2:51][CH2:52][CH3:53]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 52832925-Decen-1-ol, (5E)-HCID 5462977Diethyl azodicarboxylateHCID 1355858974-[5-[(5,5,6,6,7,7,8,8,8-Nonafluorooctyl)oxy]-2-pyrimidinyl]phenol

생성물 1

HCID 235091492-[4-[(5E)-5-Decen-1-yloxy]phenyl]-5-[(5,5,6,6,7,7,8,8,8-nonafluorooctyl)oxy]pyrimidine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of DEAD (0.261 g, 1.50 mmol) in THF (20) was added dropwise to a stirred solution of 4-[5-(5,5,6,6,7,7,8,8,8-nonafluorooctyloxy)-pyrimidin-2-yl]-phenol (0.693 g, 1.50 mmol), trans-5-decen-1-ol (0.234 g, 1.50 mmol) and triphenylphosphine (0.399 g, 1.50 mmol) in THF (30) and the reaction mixture stirred at room temperature for 16 h. The solvent was removed in vacuo and the residues purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (4:1)] to yield a colorless solid, which was recrystallized from ethanol.

후처리

  1. customThe solvent was removed in vacuo
  2. customthe residues purified by column chromatography [silica gel, eluted with hexane/ethyl acetate (4:1)]
  3. customto yield a colorless solid, which
  4. customwas recrystallized from ethanol

출처 및 근거

ORD 기록
ord-104789d05eba48a690decbce1e4e773a
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06759101B2

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