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Hydrochloric Acid → 2-(3-chloro-4,5-dihydro-1,2-oxazol-5-yl)-2-(9H-fluoren-9-ylmethoxycarbonylamino)acetic acid

HRID 127797
ノート
印刷プレビュー

反応式

HRID 127797 の反応式
[CH2:1]1[C:5]([Cl:6])=[N:4][O:3][C@@H:2]1[C@H:7]([NH2:11])[C:8]([OH:10])=[O:9].[C:12](=[O:15])(O)[O-:13].[Na+].O[CH2:18][CH:19]1[C:31]2[C:30](C(Cl)=O)=[CH:29][CH:28]=[CH:27][C:26]=2[C:25]2[C:20]1=[CH:21][CH:22]=[CH:23][CH:24]=2.Cl>C(OCC)(=O)C.O>[Cl:6][C:5]1[CH2:1][CH:2]([CH:7]([NH:11][C:12]([O:13][CH2:18][CH:19]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:25]=3[C:26]3[C:31]2=[CH:30][CH:29]=[CH:28][CH:27]=3)=[O:15])[C:8]([OH:10])=[O:9])[O:3][N:4]=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 313Hydrochloric AcidHCID 294641AcivicinHCID 516892Sodium BicarbonateHCID 86737604HCID 86737604、化合物

生成物 1

HCID 3323662-(3-chloro-4,5-dihydro-1,2-oxazol-5-yl)-2-(9H-fluoren-9-ylmethoxycarbonylamino)acetic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To 178 mg. of AT-125 in 4 ml. of water is added 300 mg. of sodium bicarbonate. After cooling the mixture to 0°-5° C., 300 mg. of 9-hydroxymethyl fluorenylcarbonyl chloride is added and it is stirred for two hours and allowed to stand overnight at room temperature. The resulting semi solid is taken up in ethyl acetate and 1 N hydrochloric acid is added until a pH of 3 is attained. The organic phase is separated, dried over sodium sulfate, concentrated and chromatographed on 20 g. of CC-4 silica gel employing 40% ethyl acetate/Hexane. Those fractions containing the desired product are evaporated and the residue recrystallized from ethyl acetate to yield 3-chloro-α-[[(9H-fluoren-9-yl-methoxy)carbonyl]amino]-4,5-dihydro-5-isoxazole acetic acid, m.p. 182°-183° C. The NMR fits the desired structure.

後処理

  1. temperatureAfter cooling the mixture to 0°-5° C.
  2. waitto stand overnight at room temperature
  3. customThe organic phase is separated
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customchromatographed on 20 g
  7. additionThose fractions containing the desired product
  8. customare evaporated
  9. customthe residue recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-249339b08d544146bf777c88eeac94ea
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04256898

反応ノート

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