Dimethyl Sulfoxide → HCID 11183809, 화합물

HRID 640525

반응식

HRID 640525 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1.CS(C)=O.[BH4-].[Na+]>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][N+:10]([O-:12])=[O:11])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 688204trans-4-Bromo-beta-nitrostyreneHCID 4311764Sodium borohydride

생성물 1

HCID 11183809HCID 11183809, 화합물수율 94.3%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of 1-bromo-4-((E)-2-nitro-vinyl)-benzene (1 g, 4.37 mmol) described in Manufacturing Example 207-1-1 in acetic acid (0.6 mL) and dimethyl sulfoxide (10 mL) was added sodium borohydride (265 mg, 6.99 mmol), which was stirred for 30 minutes at room temperature. The mixture was cooled with ice water and partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (948 mg). The title compound was used in the following reaction without any further purification.

후처리

  1. custompartitioned into ethyl acetate and water
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-b79ffe7803634152a8e738fca58caf0c
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691882B2

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