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Lithium Hexamethyldisilazide → HCID 86298931, 화합물

HRID 1428928
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HRID 1428928 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=3)[C:11](=[O:20])[NH:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.Br[CH2:32][C:33]([N:35]([CH3:46])[C:36]1[CH:45]=[CH:44][C:39]2[N:40]=[C:41]([CH3:43])[O:42][C:38]=2[CH:37]=1)=[O:34]>C1COCC1.O>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:18][CH3:19])=[CH:15][CH:16]=3)[C:11](=[O:20])[N:10]([CH2:32][C:33]([N:35]([CH3:46])[C:36]3[CH:45]=[CH:44][C:39]4[N:40]=[C:41]([CH3:43])[O:42][C:38]=4[CH:37]=3)=[O:34])[N:9]=2)[CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 2733832Lithium HexamethyldisilazideHCID 904181412-bromo-N-methyl-N-(2-methylbenzo[d]oxazol-6-yl)acetamideHCID 904187044-(3-fluorophenyl)-7-methoxyphthalazin-1(2H)-one

생성물 1

HCID 86298931HCID 86298931, 화합물수율 74.4%

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회

실험 절차

A 0° C. solution of 4-(3-fluorophenyl)-7-methoxyphthalazin-1(2H)-one (7.0 g, 25.9 mmol) in THF (160 mL) was treated with LiHMDS (1M in THF) (38 mL, 38 mmol) and stirred for 30 min. 2-Bromo-N-methyl-N-(2-methylbenzo[d]oxazol-6-yl)acetamide (7.33 g, 25.9 mmol) in THF (40 mL) was added dropwise and stirring was maintained at rt for 16 h. The reaction mixture was diluted with water (200 mL) and the product extracted with EtOAc (3×150 mL). The organics were washed with brine (100 mL), dried over Na2SO4, and concentrated. The crude was triturated with MeOH (250 mL) to yield 2-(4-(3-fluorophenyl)-7-methoxy-1-oxophthalazin-2(1H)-yl)-N-methyl-N-(2-methylbenzo[d]oxazol-6-yl)acetamide (9.1 g, 74%). (472.87 [M+H]) 1H NMR: (400 MHz, DMSO) δ: 2.62 (s, 3H), 3.33 (s, 3H), 4.95 (s, 3H), 4.73 (s, 2H), 7.37-7.43 (m, 4H), 7.48-7.51 (d, J=2.4, 8.8, 1H), 7.58-7.73 (m, 4H), 7.90 (s, 1H).

후처리

  1. stirringstirring
  2. extractionthe product extracted with EtOAc (3×150 mL)
  3. washThe organics were washed with brine (100 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customThe crude was triturated with MeOH (250 mL)

출처 및 근거

ORD 기록
ord-b3b7106aed294b88b4ee192ffead3bd8
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08937178B2

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