Ethanol → HCID 67469341, 화합물

HRID 630420노트

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HRID 630420 반응식
[NH2:1][C:2]1[C:11]([C:12]#[N:13])=[CH:10][C:5]([C:6](OC)=[O:7])=[C:4]([O:14][CH3:15])[CH:3]=1.[BH4-].[Li+].C(O)C.[Cl-].[NH4+]>O1CCCC1>[NH2:1][C:2]1[CH:3]=[C:4]([O:14][CH3:15])[C:5]([CH2:6][OH:7])=[CH:10][C:11]=1[C:12]#[N:13]

참가 물질

6

반응물 4

HCID 702EthanolHCID 25517Ammonium ChlorideHCID 4148881Lithium borohydrideHCID 67469370HCID 67469370, 화합물2회

생성물 1

HCID 67469341HCID 67469341, 화합물수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 4-amino-5-cyano-2-methoxybenzoate (intermediate 129; 0.59 g, 2.88 mmol) in tetrahydrofuran (40 mL) was added dropwise lithium tetrahydroborate 2M (21.7 mL, 43.4 mmol) at 0° C. under nitrogen atmosphere. After 5 minutes was added dropwise ethanol (7.5 mL). The mixture was stirred for five days at room temperature. Then the crude was poured into a saturated solution of ammonium chloride and ice, and stirred for 10 minutes. The crude was extracted with ethyl acetate and washed with water and brine, dried and the solvent was removed under reduced pressure to obtain the title compound as a white solid (81%).

후처리

  1. stirringstirred for 10 minutes
  2. extractionThe crude was extracted with ethyl acetate
  3. washwashed with water and brine
  4. customdried
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-c8ffdd81473c452e8f24b46e9006343c
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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