Ethanol → 2-Hydroxyethyl 2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-3,4-dihydro-2H-1-benzopyran-6-yl butanedioate

HRID 442601ノート

反応式

HRID 442601 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][C:10]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH2:18][OH:19])=[O:15])=[O:11])[C:5]([CH3:20])=[C:4]2[CH2:21][CH2:22][C:23]([CH2:26][CH2:27][CH2:28][CH:29]([CH2:31][CH2:32][CH2:33][CH:34]([CH2:36][CH2:37][CH2:38][CH:39]([CH3:41])[CH3:40])[CH3:35])[CH3:30])([CH3:25])[O:24][C:3]=12.[CH3:42][CH2:43]/[C:44](/[C:65]1[CH:70]=[CH:69][CH:68]=[CH:67][CH:66]=1)=[C:45](/[C:52]1[CH:57]=[CH:56][C:55]([O:58][CH2:59][CH2:60][N+:61](C)([CH3:63])[CH3:62])=[CH:54][CH:53]=1)\[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1.[I-:71].[CH2:72](O)C.O=[Si]=O>O>[CH3:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][C:10]([CH2:12][CH2:13][C:14]([O:16][CH2:17][CH2:18][OH:19])=[O:15])=[O:11])[C:5]([CH3:20])=[C:4]2[CH2:21][CH2:22][C:23]([CH2:26][CH2:27][CH2:28][CH:29]([CH2:31][CH2:32][CH2:33][CH:34]([CH2:36][CH2:37][CH2:38][CH:39]([CH3:41])[CH3:40])[CH3:35])[CH3:30])([CH3:25])[O:24][C:3]=12.[CH3:42][CH2:43]/[C:44](/[C:65]1[CH:66]=[CH:67][CH:68]=[CH:69][CH:70]=1)=[C:45](/[C:52]1[CH:53]=[CH:54][C:55]([O:58][CH2:59][CH2:60][N:61]([CH3:63])[CH3:62])=[CH:56][CH:57]=1)\[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=1.[CH3:72][I:71]

参加物

7

反応物 4

HCID 702EthanolHCID 24261SilicaHCID 714062-Hydroxyethyl 2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-3,4-dihydro-2H-1-benzopyran-6-yl butanedioateHCID 3033898Ethanaminium, 2-(4-((1Z)-1,2-diphenyl-1-buten-1-yl)phenoxy)-N,N,N-trimethyl-, iodide (1:1)

生成物 2

HCID 714062-Hydroxyethyl 2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)-3,4-dihydro-2H-1-benzopyran-6-yl butanedioateHCID 21150887Tamoxifen methyliodide

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

TPGS (500 mg) was melted at 40°-60° C. in a water bath. Tamoxifen methiodide (100 mg, from Pharmos Corp., FL., USA) was added to the melted material and the mixture was agitated for several minutes. A small amount of absolute ethanol (up to 5%, v/v) was added in order to get an homogeneous mixture. PVP (Kollidon PF 12, 2.6 ml of a 10% solution in water) was then added and the mixture was agitated again for several minutes. Cab-O-Sil (2.8 ml of a 5% solution in water) was added and the mixture was agitated again for several minutes. The resultant TPGS/PVP/Tamoxifen methiodide mixture was then freeze-dried overnight using a Christ beta lyophilizer (Germany). A powdered free-flowing TPGS/PVP/Tamoxifen methyliodide coprecipitate quickly dispersible in water was obtained.

後処理

  1. customto get an homogeneous mixture
  2. stirringthe mixture was agitated again for several minutes
  3. stirringthe mixture was agitated again for several minutes
  4. dry with materialThe resultant TPGS/PVP/Tamoxifen methiodide mixture was then freeze-dried overnight

出典と根拠

ORDレコード
ord-300adfcd2094433eafaa2254c9b76d4a
出典データセット
uspto-grants-1999_04
特許番号
US05891469

反応ノート

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