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Water → [7-Chloro-9-(4-methylpiperazin-1-ylmethyl)-2,3-dihydro-[1,4]dioxino[2,3-g]quinolin-8-yl]-methanol

HRID 411841
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HRID 411841 반응식
O.C[O:3][C:4]([C:6]1[C:7]([Cl:28])=[N:8][C:9]2[CH:10]=[C:11]3[O:27][CH2:26][CH2:25][O:24][C:12]3=[CH:13][C:14]=2[C:15]=1[CH2:16][N:17]1[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]1)=O.[H-].C([Al+]CC(C)C)C(C)C.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C(Cl)Cl>[Cl:28][C:7]1[C:6]([CH2:4][OH:3])=[C:15]([CH2:16][N:17]2[CH2:18][CH2:19][N:20]([CH3:23])[CH2:21][CH2:22]2)[C:14]2[CH:13]=[C:12]3[O:24][CH2:25][CH2:26][O:27][C:11]3=[CH:10][C:9]=2[N:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 9357Potassium Sodium TartrateHCID 154504617-Chloro-9-(4-methylpiperazin-1-ylmethyl)-2,3-dihydro[1,4]dioxino[2,3-g]quinoline-8-carboxylic acid methyl ester2회HCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 22637071[7-Chloro-9-(4-methylpiperazin-1-ylmethyl)-2,3-dihydro-[1,4]dioxino[2,3-g]quinolin-8-yl]-methanol

시약·촉매·용매

1
HCID 6344Dichloromethane용매2회

실험 절차

A 4-necked 5-L round-bottom flask is equipped with an overhead mechanical stirrer, a water-cooled condenser and nitrogen flow is maintained. The flask is charged with 7-chloro-9-(4-methylpiperazin-1-ylmethyl)-2,3-dihydro[1,4]dioxino [2,3-g]quinoline-8-carboxylic acid methyl ester (Intermediate 7, 194 g, 495 mol), as a solution in 1 L of methylene chloride. To the solution is added 1 M diisobutylaluminum hydride in methylene chloride (2.00 L, 2.00 mol) over 15 min. The solution is heated to reflux during the addition. The reaction is allowed to cool to ambient temperature and stirred for 4 h. The reaction mixture is transferred to a 15-L separatory funnel containing a saturated solution of Rochelle's salt (5 L). After being stirred for 2.5 h, the organic layer is separated and the aqueous layer is extracted with methylene chloride (3×2.5 L). The combined organic layers are washed with brine (3 L), dried over anhydrous sodium sulfate and concentrated in vacuo. The resultant thick brown slurry is successively treated with methylene chloride (500 mL) and hexane (1 L). The mixture is swirled at 0° C. for 30 min. The precipitate is collected on a Buchner funnel, washed with 1 liter of hexane and dried in vacuo. at 30° C. yielding [7-chloro-9-(4-methylpiperazin-1-ylmethyl)-2,3-dihydro-[1,4]dioxino[2,3-g]quinolin-8-yl]-methanol as a yellow crystalline solid: mp 178-180° C. 1H NMR (CDCl3, 200 MHz) d 2.26 (s, 3H), 2.63 (br. s, 4H), 4.00 (s, 2H). 4.39(s, 4H), 4.93 (s, 2H), 6.10 (br. s, 1H), 7.46 (s, 1H), 7.51 (s, 1H). Elemental analysis: Calculated for C18H22ClN3O3: C, 59.42; H, 6.09; N, 11.55. Found: C, 59.41; H, 6.12; N, 11.46.

후처리

  1. customA 4-necked 5-L round-bottom flask is equipped with an overhead mechanical stirrer
  2. temperaturenitrogen flow is maintained
  3. temperatureThe solution is heated
  4. temperatureto reflux during the addition
  5. customThe reaction mixture is transferred to a 15-L separatory funnel
  6. stirringAfter being stirred for 2.5 h
  7. customthe organic layer is separated
  8. extractionthe aqueous layer is extracted with methylene chloride (3×2.5 L)
  9. washThe combined organic layers are washed with brine (3 L)
  10. dry with materialdried over anhydrous sodium sulfate
  11. concentrationconcentrated in vacuo
  12. additionThe resultant thick brown slurry is successively treated with methylene chloride (500 mL) and hexane (1 L)
  13. waitThe mixture is swirled at 0° C. for 30 min
  14. customThe precipitate is collected on a Buchner funnel
  15. washwashed with 1 liter of hexane
  16. customdried in vacuo

출처 및 근거

ORD 기록
ord-92f82e47ae1b44559470fef87bf13071
출처 데이터셋
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06559309B2

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