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Benzyl Alcohol → HCID 67670349、化合物

HRID 1417552
ノート
印刷プレビュー

反応式

HRID 1417552 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C@H:8]2[C@@H:33](C(O)=O)[CH2:32][CH2:31][C@@:9]32[O:13][CH2:12][C@H:11]([C:14]2[CH:19]=[C:18]([N:20]4[CH:24]=[CH:23][N:22]=[C:21]4[C:25]([F:28])([F:27])[F:26])[CH:17]=[CH:16][C:15]=2[O:29][CH3:30])[CH2:10]3)=[CH:4][CH:3]=1.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:44])C=CC=CC=1.C([N:57]([CH:60](C)C)CC)(C)C.[CH2:63]([OH:70])[C:64]1[CH:69]=[CH:68][CH:67]=[CH:66][CH:65]=1>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH2:63]([O:70][C:60]([NH:57][C@H:33]1[CH2:32][CH2:31][C@:9]2([O:13][CH2:12][C@H:11]([C:14]3[CH:19]=[C:18]([N:20]4[CH:24]=[CH:23][N:22]=[C:21]4[C:25]([F:26])([F:27])[F:28])[CH:17]=[CH:16][C:15]=3[O:29][CH3:30])[CH2:10]2)[C@@H:8]1[C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)=[O:44])[C:64]1[CH:69]=[CH:68][CH:67]=[CH:66][CH:65]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 244Benzyl AlcoholHCID 81531DiisopropylethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 67672163HCID 67672163、化合物

生成物 1

HCID 67670349HCID 67670349、化合物収率 62%

試薬・触媒・溶媒 2

HCID 1140Toluene
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of (3S,5R,6R,7S)-6-(4-fluorophenyl)-3-(2-methoxy-5-(2-(trifluoromethyl)imidazol-1-yl)phenyl)-1-oxaspiro[4.4]nonane-7-carboxylic acid (40 mg, 0.079 mmol), diphenylphosphoryl azide (24 mg, 0.08 mmol), and diisopropylethylamine (0.017 mL, 0.095 mmol) in toluene was stirred at RT for 0.5 h, and then heated at 100° C. for 50 min. After addition of benzyl alcohol (0.5 mL), the mixture was heated at 100° C. overnight. Upon cooling to RT, the mixture was taken up in 25 mL of ethyl acetate and washed successively with 15 mL of saturated aqueous sodium bicarbonate and 15 mL of brine. Drying over sodium sulfate and evaporation afforded the crude product, which was purified by column chromatography, eluting with 3-5% ethyl acetate in dichloromethane, to give the title compound (30 mg, 62%) as a light brown syrup. Mass spectrum (NH3/CI): m/z=610.1 (M+1).

後処理

  1. temperatureheated at 100° C. for 50 min
  2. temperaturethe mixture was heated at 100° C. overnight
  3. temperatureUpon cooling to RT
  4. washwashed successively with 15 mL of saturated aqueous sodium bicarbonate and 15 mL of brine
  5. dry with materialDrying over sodium sulfate and evaporation
  6. customafforded the crude product, which
  7. customwas purified by column chromatography
  8. washeluting with 3-5% ethyl acetate in dichloromethane

出典と根拠

ORDレコード
ord-7545a134aa56488fad6e2c7d49db0547
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05877191

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート