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Hexane → 2-[2-(4-Methoxycarbonylmethylphenoxy)-1(R)-methylethyl]amino-1(R)-(3-chlorophenyl)ethanol fumarate

HRID 1682730
ノート
印刷プレビュー

反応式

HRID 1682730 の反応式
CCCCCC.[CH3:7][O:8][C:9]([CH2:11][C:12]1[CH:32]=[CH:31][C:15]([O:16][CH2:17][C@H:18]([NH:20][CH2:21][C@@H:22]([C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[CH:25]=2)[OH:23])[CH3:19])=[CH:14][CH:13]=1)=[O:10].[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]/[C:36]([OH:38])=[O:37]>C(OCC)(=O)C>[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]/[C:36]([OH:38])=[O:37].[CH3:7][O:8][C:9]([CH2:11][C:12]1[CH:32]=[CH:31][C:15]([O:16][CH2:17][C@H:18]([NH:20][CH2:21][C@@H:22]([C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([Cl:30])[CH:25]=2)[OH:23])[CH3:19])=[CH:14][CH:13]=1)=[O:10]
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 8058HexaneHCID 444972Fumaric AcidHCID 228670762-[2-(4-methoxycarbonylmethylphenoxy)-1(R)methylethyl]amino-1(R)-(3-chlorophenyl)ethanol

生成物 1

HCID 228731262-[2-(4-Methoxycarbonylmethylphenoxy)-1(R)-methylethyl]amino-1(R)-(3-chlorophenyl)ethanol fumarate収率 93.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate
溶媒

実験手順

30 ml of hexane were slowly added to a solution of 1.6 g of 2-[2-(4-methoxycarbonylmethylphenoxy)-1(R)methylethyl]amino-1(R)-(3-chlorophenyl)ethanol (prepared as described in Example 46) and 491 mg of fumaric acid in 5 ml of ethyl acetate, whilst irradiating the reaction mixture with ultrasonic waves. The crystals which precipitated were collected by filtration and dried, to give 1.95 g of the title compound as crystals, melting at 73°-78° C. [α]D23 -19.4° (c=1.01, methanol).

後処理

  1. customwhilst irradiating the reaction mixture with ultrasonic waves
  2. customThe crystals which precipitated
  3. filtrationwere collected by filtration
  4. customdried

出典と根拠

ORDレコード
ord-719a3e26b8a8497c8557909e3baff067
出典データセット
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05635534

反応ノート

読み込み中…

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