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HCID 11323174、化合物 → HCID 54497369、化合物

HRID 2187422
ノート
印刷プレビュー

反応式

HRID 2187422 の反応式
[F:1][C:2]([F:17])([F:16])[S:3]([O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([OH:15])=O)=[CH:9][CH:8]=1)(=[O:5])=[O:4].[NH2:18][C@@H:19]1[CH2:28][CH2:27][C:26]2[C:21](=[C:22]([N:29]3[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][CH2:30]3)[CH:23]=[CH:24][CH:25]=2)[CH2:20]1>S(Cl)(Cl)=O.C(Cl)Cl>[CH3:35][N:32]1[CH2:33][CH2:34][N:29]([C:22]2[CH:23]=[CH:24][CH:25]=[C:26]3[C:21]=2[CH2:20][C@H:19]([NH:18][C:13](=[O:15])[C:10]2[CH:9]=[CH:8][C:7]([O:6][S:3]([C:2]([F:1])([F:17])[F:16])(=[O:4])=[O:5])=[CH:12][CH:11]=2)[CH2:28][CH2:27]3)[CH2:30][CH2:31]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 11323174HCID 11323174、化合物HCID 53960413(R)-2-amino-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalene

生成物 1

HCID 54497369HCID 54497369、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 24386Thionyl Chloride溶媒

反応条件

温度
40 °C

実験手順

4-Carboxyphenyl trifluoromethanesulfonate (0.40 g, 1.5 mmol; described in: Looker, J. H.; Hayes, C. H.; Thatcher, D. N. J. Am. Chem. Soc. 1957, 79, 741-4) was dissolved in thionyl chloride (10 mL) and heated at 40° C. for 45 min. The excess of thionyl chloride was evaporated in vacuo, the residue was treated with toluene and again the solvent was removed in vacuo. The crude acid chloride (280 mg, 0.96 mmol) was dissolved in methylene chloride (5 mL) and added dropwise to an ice-cooled solution of (R)-2-amino-8-(4-methylpiperazin-1-yl)-1,2,3,4-tetrahydronaphthalene (110 mg, 0.46 mmol) and triethylarine (96 μL, 0.69 mmol) in methylene chloride (20 mL). After the addition the reaction was allowed to stir at ambient temperature for 15 min and then washed with water. The phases were separated and the combined organic phases were dried (Na2SO4), filtered and evaporated in vacuo to give a crude product which was purified on a silica gel column using chloroform/ethanol saturated with NH3 (100:3) as the eluent. Yield: 100 mg (44%) of the title compound as white crystals: mp 178-180° C.; [α]21D −31° (c 1.0, chloroform); EIMS (70 eV) m/z (relative intensity) 497 (17, M+).

後処理

  1. customThe excess of thionyl chloride was evaporated in vacuo
  2. additionthe residue was treated with toluene
  3. customagain the solvent was removed in vacuo
  4. additionAfter the addition the reaction
  5. washwashed with water
  6. customThe phases were separated
  7. dry with materialthe combined organic phases were dried (Na2SO4)
  8. filtrationfiltered
  9. customevaporated in vacuo

出典と根拠

ORDレコード
ord-d6916291e19745889e73c92b421f12d9
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06410530B1

反応ノート

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