alpha-Methyltryptophan → HCID 68849237、化合物

HRID 2275397

反応式

HRID 2275397 の反応式
[CH3:1][C:2]([C:14](O)=[O:15])([CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)[NH2:3]>C1COCC1>[NH2:3][C:2]([CH3:1])([CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:7][CH:6]=1)[CH2:14][OH:15]

参加物

3

反応物 1

HCID 95438alpha-Methyltryptophan

生成物 1

HCID 68849237HCID 68849237、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
65 °C

実験手順

To a solution of alpha-methyl-DL-tryptophan (100 mg) in dry THF (10 ml) was added a borane-tetrahydrofuran complex (1.14 ml) dropwise. The reaction mixture was heated at 65° C. for 4.5 hours. The reaction mixture was quenched with ethanol (3 ml). The reaction mixture was concentrated and extracted with ethyl acetate and water. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by preparative HPLC eluting with acetonitrile and water. The pure fractions were collected and freezedried.

後処理

  1. customThe reaction mixture was quenched with ethanol (3 ml)
  2. concentrationThe reaction mixture was concentrated
  3. extractionextracted with ethyl acetate and water
  4. dry with materialThe organic layer was dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by preparative HPLC
  8. washeluting with acetonitrile and water
  9. customThe pure fractions were collected
  10. customfreezedried

出典と根拠

ORDレコード
ord-0fb0c1dc1df1450daeb532bb4f95ee12
出典データセット
uspto-grants-2015_09
特許番号
US09127007B2

関連ノート

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