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Sodium Hydroxide → HCID 53988844、化合物

HRID 482280
ノート
印刷プレビュー

反応式

HRID 482280 の反応式
[CH:1]1([CH2:4][O:5][C:6]2[CH:11]=[CH:10][C:9]([CH2:12][N:13]3[CH2:18][CH2:17][CH:16]([C:19]([C:31]4[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:39])[F:38])=[CH:33][CH:32]=4)([C:21]4[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=4)[OH:20])[CH2:15][CH2:14]3)=[CH:8][CH:7]=2)[CH2:3][CH2:2]1.ClC1C=C(C=CC=1)C(OO)=[O:46].[OH-].[Na+]>C(Cl)Cl>[CH:1]1([CH2:4][O:5][C:6]2[CH:7]=[CH:8][C:9]([CH2:12][N+:13]3([O-:46])[CH2:14][CH2:15][CH:16]([C:19]([C:21]4[CH:26]=[CH:25][C:24]([C:27]([F:29])([F:28])[F:30])=[CH:23][CH:22]=4)([C:31]4[CH:36]=[CH:35][C:34]([C:37]([F:40])([F:38])[F:39])=[CH:33][CH:32]=4)[OH:20])[CH2:17][CH2:18]3)=[CH:10][CH:11]=2)[CH2:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 11837562N-[4-(cyclopropylmethoxy)phenylmethyl]-4-[bis(4-trifluoromethylphenyl)hydroxymethyl]piperidine

生成物 1

HCID 53988844HCID 53988844、化合物収率 97.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of 10.0 grams (0.018 mole) of N-[4-(cyclopropylmethoxy)phenylmethyl]-4-[bis(4-trifluoromethylphenyl)hydroxymethyl]piperidine in methylene chloride was cooled to 0° C., and 3.1 grams (0.01 2 mole) of 50% 3-chloroperoxybenzoic acid was added in two portions. Upon completion of the addition the reaction mixture was allowed to warm to ambient temperature, where it stirred for about 18 hours. After this time, the reaction mixture was poured into aqueous 5% sodium hydroxide solution. The organic layer was separated and washed with aqueous 5% sodium hydroxide solution. The organic layer was then filtered through phase separated silicone treated paper. The filtrate was concentrated under reduced pressure, yielding 10.2 grams of N-[4-(cyclopropylmethoxy)phenylmethyl]-4-[bis(4-trifluoromethylphenyl)hydroxy-methyl]piperidine N-oxide. The NMR spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of the addition the reaction mixture
  2. customThe organic layer was separated
  3. washwashed with aqueous 5% sodium hydroxide solution
  4. filtrationThe organic layer was then filtered through phase
  5. customseparated silicone treated paper
  6. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-89eac9321f9f4be8bff49b44e4243d5d
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05795901

反応ノート

読み込み中…

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