Hydrochloric Acid → HCID 59288344、化合物

HRID 2420637ノート

反応式

HRID 2420637 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH:12]([C:18](OCC)=[O:19])[C:13](OCC)=[O:14])[O:8][CH2:7][CH:6]([CH2:23][CH2:24][CH3:25])[CH2:5]2.[H-].C([Al+]CC(C)C)C(C)C.Cl>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[CH:12]([CH2:18][OH:19])[CH2:13][OH:14])[O:8][CH2:7][CH:6]([CH2:23][CH2:24][CH3:25])[CH2:5]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21225700DiisobutylaluminumhydrideHCID 59288369HCID 59288369、化合物

生成物 1

HCID 59288344HCID 59288344、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

8.7 g (21.1 mmol) of the diethyl 2-(6-fluoro-3-propylchroman-7-yl)malonate obtained under 1.2. are initially introduced in 60 ml of toluene, and 106 ml (106 mmol) of a 1 M solution of diisobutylaluminium hydride in toluene are added dropwise at 5° C. The batch is subsequently added to ice-cold sat. ammonium chloride soln., acidified using dil. hydrochloric acid and extracted with MTB ether. The combined org. phases are dried over sodium sulfate and evaporated. Chromatography of the crude product on silica gel with MTB ether/heptane (4:1) gives 2-(6-fluoro-3-propylchroman-7-yl)propane-1,3-diol as a colourless solid.

後処理

  1. additionThe batch is subsequently added to ice-cold sat. ammonium chloride soln
  2. extractionextracted with MTB ether
  3. dry with materialphases are dried over sodium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-eb90ce9974ac4472a69af2a9bfcbb89c
出典データセット
uspto-grants-2011_06
特許番号
US07955664B2

反応ノート

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