Bromotrimethylsilane → (1S,5S)-(1-{5-[(4-amino-benzenesulfonyl)-isobutyl-amino]-6-phosphonooxy hexylcarbamoyl}-2,2-diphenyl-ethyl)-carbamic acid methyl ester

HRID 1516423

反応式

HRID 1516423 の反応式
[CH3:1][O:2][C:3](=[O:52])[NH:4][C@H:5]([C:19](=[O:51])[NH:20][CH2:21][CH2:22][CH2:23][CH2:24][C@H:25]([N:36]([S:41]([C:44]1[CH:49]=[CH:48][C:47]([NH2:50])=[CH:46][CH:45]=1)(=[O:43])=[O:42])[CH2:37][CH:38]([CH3:40])[CH3:39])[CH2:26][O:27][P:28]([O:33]CC)([O:30]CC)=[O:29])[CH:6]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.C[Si](Br)(C)C>ClCCl>[CH3:1][O:2][C:3](=[O:52])[NH:4][C@H:5]([C:19](=[O:51])[NH:20][CH2:21][CH2:22][CH2:23][CH2:24][C@H:25]([N:36]([S:41]([C:44]1[CH:45]=[CH:46][C:47]([NH2:50])=[CH:48][CH:49]=1)(=[O:42])=[O:43])[CH2:37][CH:38]([CH3:40])[CH3:39])[CH2:26][O:27][P:28]([OH:33])([OH:30])=[O:29])[CH:6]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 24778259(1S,5S)-{1-[5-[(4-amino-benzenesulfonyl)-isobutyl-amino]-6-(diethoxy-phosphoryloxy)-hexylcarbamoyl]-2,2-diphenyl-ethyl}-carbamic acid methyl ester

生成物 1

HCID 11563875(1S,5S)-(1-{5-[(4-amino-benzenesulfonyl)-isobutyl-amino]-6-phosphonooxy hexylcarbamoyl}-2,2-diphenyl-ethyl)-carbamic acid methyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The product of step G prepared above (152 mg) was dissolved in anhydrous dichloromethane (3.0 mL). Trimethylsilyl bromide (0.5 mL) was added at 0° C. The mixture was stirred during 1 h at this temperature and overnight at room temperature. The solvent was evaporated and 0.2 mL water was added to the residue. 3 mL EtOH was added mixed and evaporated. This step was repeated three times and the residue dried in vacuo. Yields 98 mg 70% of the title derivatives of this first example.

後処理

  1. customThe solvent was evaporated
  2. addition0.2 mL water was added to the residue
  3. addition3 mL EtOH was added
  4. additionmixed
  5. customevaporated
  6. customthe residue dried in vacuo
  7. customYields 98 mg 70% of the title derivatives of this first example

出典と根拠

ORDレコード
ord-196f3ad9995f4b0da2bdd77d30eb1d4b
出典データセット
uspto-grants-2012_07
特許番号
US08227450B2

関連ノート

読み込み中…