Sodium Hydroxide → HCID 21387541, 화합물

HRID 1833853노트

반응식

HRID 1833853 반응식
[BH4-].[Na+].[Cl:3][C:4]1[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=1[C:6]([C:8]1[O:9][CH:10]=[CH:11][CH:12]=1)=[O:7].[OH-].[Na+]>CO.O>[Cl:3][C:4]1[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=1[CH:6]([C:8]1[O:9][CH:10]=[CH:11][CH:12]=1)[OH:7]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 21387596(2-Chlorophenyl)(furan-2-yl)methanone

생성물 1

HCID 21387541HCID 21387541, 화합물수율 70.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Portions of sodium borohydride (total 15 g.) were added over an hour to a stirred solution of 2-(2-chlorobenzoyl)furan (prepared as hereinbefore described; 100 g.) in methanol (500 ml.) at 10°-25° C. After stirring for 1 hour, the solution was heated briefly to the boiling point and, when effervescence had ceased, sodium hydroxide solution (2N, 100 ml.) was added. The solution was heated at reflux for 30 minutes, diluted with water (1 liter) and extracted with diethyl ether (4 × 150 ml.). The combined extracts were washed with water (2 × 100 ml.), dried over sodium sulphate, filtered and evaporated to a clear oil, which was distilled to give (±) 2-(2-chloro-α-hydroxybenzyl)furan (71 g.), b.p. 136° C./0.1 mm.Hg, as a viscous yellow oil.

후처리

  1. temperaturethe solution was heated briefly to the boiling point and, when effervescence
  2. temperatureThe solution was heated
  3. temperatureat reflux for 30 minutes
  4. extractionextracted with diethyl ether (4 × 150 ml.)
  5. washThe combined extracts were washed with water (2 × 100 ml.)
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated to a clear oil, which
  9. distillationwas distilled

출처 및 근거

ORD 기록
ord-0d5304bca913410ca35ccfe53ed52d6d
출처 데이터셋
uspto-grants-1978_01
특허 번호
US04067723

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