Benzyl Alcohol → HCID 13255306, 화합물

HRID 903977노트

반응식

HRID 903977 반응식
[CH3:1][O:2][C:3]1[C:4](=[O:18])[C:5]2[C:10]([C:11](=[O:15])[C:12]=1[O:13][CH3:14])=[C:9]([C:16]#[N:17])[CH:8]=[CH:7][CH:6]=2.C(O)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>O1CCCC1>[CH2:1]([O:2][C:3]1[C:4](=[O:18])[C:5]2[C:10]([C:11](=[O:15])[C:12]=1[O:13][CH2:14][C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)=[C:9]([C:16]#[N:17])[CH:8]=[CH:7][CH:6]=2)[C:3]1[CH:4]=[CH:5][CH:10]=[CH:11][CH:12]=1

참가 물질

4

반응물 2

HCID 244Benzyl AlcoholHCID 132552666,7-Dimethoxy-5,8-dioxo-5,8-dihydronaphthalene-1-carbonitrile

생성물 1

HCID 13255306HCID 13255306, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

14b From Example 9 (972 mg, 4 mmol) is dissolved in tetrahydrofuran (100 ml) containing benzyl alcohol (8 ml) and the tetrahydrofuran (40 ml) is distilled off. The remaining solution is cooled to 15° and sodium hydride (5 mg) with 3 A molecular sieve (2 g) is added. The resulting mixture is stirred at 15°-20° for 20 minutes. The mixture is filtered through a celite bed, the filtrate concentrated to dryness and the residue crystallized from isopropanol giving 1.01 g (64%) of 23 with mp 118°-121°.

후처리

  1. distillationthe tetrahydrofuran (40 ml) is distilled off
  2. temperatureThe remaining solution is cooled to 15°
  3. additionsodium hydride (5 mg) with 3 A molecular sieve (2 g) is added
  4. filtrationThe mixture is filtered through a celite bed
  5. concentrationthe filtrate concentrated to dryness
  6. customthe residue crystallized from isopropanol giving 1.01 g (64%) of 23 with mp 118°-121°

출처 및 근거

ORD 기록
ord-353a5ea894b54e4b8827b3378485dcf5
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04229478

반응 노트

불러오는 중…