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Sodium bis(trimethylsilyl)amide → 6-(2,4,6-Trifluorophenyl)pyrido[2,3-c]pyridazine-5,7(6H,8H)-dione

HRID 2217967
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HRID 2217967 반응식
C(O[C:4]([C:6]1[CH:11]=[CH:10][N:9]=[N:8][C:7]=1[NH:12][C:13](=[O:24])[CH2:14][C:15]1[C:20]([F:21])=[CH:19][C:18]([F:22])=[CH:17][C:16]=1[F:23])=[O:5])C.C[Si]([N-][Si](C)(C)C)(C)C.[Na+]>C1COCC1>[F:21][C:20]1[CH:19]=[C:18]([F:22])[CH:17]=[C:16]([F:23])[C:15]=1[CH:14]1[C:13](=[O:24])[NH:12][C:7]2[N:8]=[N:9][CH:10]=[CH:11][C:6]=2[C:4]1=[O:5]
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참가 물질

4

반응물 2

HCID 2724254Sodium bis(trimethylsilyl)amideHCID 68934065HCID 68934065, 화합물

생성물 1

HCID 597692086-(2,4,6-Trifluorophenyl)pyrido[2,3-c]pyridazine-5,7(6H,8H)-dione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

The product from Step 2 (2.0 g) was dissolved in dry THF (50 ml), and sodium bis-trimethylsilylamide (17.7 ml of a 11.0M solution in THF) was added dropwise with stirring under nitrogen at 0° C. The reaction was stirred for 3 hours at 0° C. and a yellow precipitate was formed. The reaction was quenched with concentrated hydrochloric acid and then poured into ice water. The solid was filtered, washed with water and air dried to give 6-(2,4,6-trifluorophenyl)-8H-pyrido[2,3-c]pyridazine-5,7-dione as a yellow solid (1.9 2 g), m.p. >330° C., still containing some THF, which was used without further purification.

후처리

  1. stirringThe reaction was stirred for 3 hours at 0° C.
  2. customa yellow precipitate was formed
  3. customThe reaction was quenched with concentrated hydrochloric acid
  4. additionpoured into ice water
  5. filtrationThe solid was filtered
  6. washwashed with water and air
  7. customdried

출처 및 근거

ORD 기록
ord-51c90b24e6004dcdbb7b8aa8c9b415bf
출처 데이터셋
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07410967B2

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