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Esomeprazolemagnesiumtrihydrate → HCID 178488035、化合物

HRID 1455534
ノート
印刷プレビュー

反応式

HRID 1455534 の反応式
[CH3:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([CH3:10])[C:5]([CH2:11][S:12]([C:14]2[N-:18][C:17]3[CH:19]=[CH:20][C:21]([O:23][CH3:24])=[CH:22][C:16]=3[N:15]=2)=[O:13])=[N:4][CH:3]=1.[CH3:25][C:26]1[C:31]([O:32][CH3:33])=[C:30]([CH3:34])[C:29]([CH2:35][S:36]([C:38]2[N-:42][C:41]3[CH:43]=[CH:44][C:45]([O:47][CH3:48])=[CH:46][C:40]=3[N:39]=2)=[O:37])=[N:28][CH:27]=1.O.O.O.[Mg+2:52]>ClCCl.CO>[CH3:1][C:2]1[CH:3]=[N:4][C:5]([CH2:11][S+:12]([O-:13])[C:14]2[N-:18][C:17]3[CH:19]=[CH:20][C:21]([O:23][CH3:24])=[CH:22][C:16]=3[N:15]=2)=[C:6]([CH3:10])[C:7]=1[O:8][CH3:9].[CH3:25][C:26]1[CH:27]=[N:28][C:29]([CH2:35][S+:36]([O-:37])[C:38]2[N-:42][C:41]3[CH:43]=[CH:44][C:45]([O:47][CH3:48])=[CH:46][C:40]=3[N:39]=2)=[C:30]([CH3:34])[C:31]=1[O:32][CH3:33].[Mg+2:52]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 130565Esomeprazolemagnesiumtrihydrate

生成物 1

HCID 178488035HCID 178488035、化合物収率 64.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

Esomeprazole magnesium trihydrate (200 g) was dissolved in a mixture of dichloromethane (1200 ml) and methanol (1200 ml) at 25-30° C., Any undissolved material was filtered off and triethylamine (2 ml) was added to the filtrate. The clear solution thus obtained was spray dried in a mini spray dryer (Model Buchi—190) with an inlet temperature of 65-68° C. and an outlet temperature of 22-42° C. in 2 to 3 hours. The solid was further dried under vacuum at 60-65° C. for 14 to 15 hours to yield 120 g of esomeprazole magnesium of amorphous form. X-ray powder diffraction pattern showed a plain halo, which demonstrates the amorphous nature of the product. The following physical characteristics were obtained: Purity 99.77% by HPLC, Chiral purity 99.90% by HPLC, SOR 145.9°, Mg content 3.4.

後処理

  1. filtrationAny undissolved material was filtered off
  2. additiontriethylamine (2 ml) was added to the filtrate
  3. customThe clear solution thus obtained
  4. customdried in a mini spray dryer (Model Buchi—190) with an inlet temperature of 65-68° C. and an outlet temperature of 22-42° C. in 2 to 3 hours
  5. customThe solid was further dried under vacuum at 60-65° C. for 14 to 15 hours

出典と根拠

ORDレコード
ord-ddceb036f0cf4b8782327ea6e9acf2fa
出典データセット
uspto-grants-2009_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07482463B2

反応ノート

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