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Acetonitrile → 1-[3-(Benzoylthio)-3-(benzo[b]thien-3-ylcarbonyl)propionyl]-L-proline

HRID 66487
ノート
印刷プレビュー

反応式

HRID 66487 の反応式
Br[CH:2]([C:14]([C:16]1[C:17]2[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=2[S:19][CH:20]=1)=[O:15])[CH2:3][C:4]([N:6]1[CH2:13][CH2:12][CH2:11][C@H:7]1[C:8]([OH:10])=[O:9])=[O:5].C(#N)C.C[O-].[Na+].[C:31]([OH:39])(=[S:38])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1>C(O)(=O)C>[C:31]([S:38][CH:2]([C:14]([C:16]1[C:17]2[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=2[S:19][CH:20]=1)=[O:15])[CH2:3][C:4]([N:6]1[CH2:13][CH2:12][CH2:11][C@H:7]1[C:8]([OH:10])=[O:9])=[O:5])(=[O:39])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6342Acetonitrile2 回HCID 10942334Sodium MethoxideHCID 536867021-[3-bromo-3-(benzo[b]thien-3-ylcarbonyl)propionyl]-L-prolineHCID 178526132HCID 178526132、化合物

生成物 1

HCID 536406471-[3-(Benzoylthio)-3-(benzo[b]thien-3-ylcarbonyl)propionyl]-L-proline

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

実験手順

As for Example 21, 1-[3-bromo-3-(benzo[b]thien-3-ylcarbonyl)propionyl]-L-proline (0.01 mole) in 25 ml. of acetonitrile is added to a mixture of 0.01 mole of sodium methoxide and 0.015 mole of thiobenzoic acid in 25 ml. of acetonitrile. The mixture is stirred at room temperature for 16 hours, one ml. of acetic acid is added and the solvent is evaporated in vacuo. The residue is partitioned between dichloromethane and water containing acetic acid. The organic layer is separated, washed with water and dried over magnesium sulfate. The solvent is removed in vacuo to give the product of the Example as a yellow glass.

後処理

  1. customthe solvent is evaporated in vacuo
  2. customThe residue is partitioned between dichloromethane and water
  3. additioncontaining acetic acid
  4. customThe organic layer is separated
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent is removed in vacuo
  8. customto give the product of the Example as a yellow glass

出典と根拠

ORDレコード
ord-d5333786507a455dbe9cc8aec7a7b339
出典データセット
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04342689

反応ノート

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