Water → 6-Chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine]

HRID 1707117ノート

反応式

HRID 1707117 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[CH2:9][C:10]3([CH2:15][CH2:14][N:13](C#N)[CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.C(O)(=O)/C=C\C(O)=O>O1CCCC1.CCOCC>[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[CH2:9][C:10]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 962WaterHCID 444266Maleic AcidHCID 131540506-Chloro-1'-cyano-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine]HCID 21226445Aluminium lithium hydride

生成物 1

HCID 128016236-Chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine]

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 3.4 g of 6-chloro-1'-cyano-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine], Example 26, in 50 ml of tetrahydrofuran is added dropwise to a refluxing slurry of 1.0 g of lithium aluminum hydride in 50 ml of tetrahydrofuran. After total addition the mixture is stirred at reflux for 2.5 hours before being treated with water and alkali. The resulting oily product, in ether, is converted to its maleic acid salt which is recrystallized from an ethyl alcohol-ether mixture to provide off-white granules, mp 174.5°-175.5° C. of 6-chloro-1-(2-fluorophenyl)spiro[indoline-3,4'-piperidine] meleate.

後処理

  1. additionAfter total addition the mixture
  2. temperatureat reflux for 2.5 hours
  3. customis recrystallized from an ethyl alcohol-ether mixture

出典と根拠

ORDレコード
ord-52b6cc80c33e4b2e937b20a61c2a5c09
出典データセット
uspto-grants-1980_06
特許番号
US04209625

反応ノート

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