Hydrochloric Acid → HCID 59288344, 화합물

HRID 2420637노트

반응식

HRID 2420637 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 21225700DiisobutylaluminumhydrideHCID 59288369HCID 59288369, 화합물

생성물 1

HCID 59288344HCID 59288344, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eb90ce9974ac4472a69af2a9bfcbb89c
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07955664B2

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