4-Methylmorpholine → Boc-gly-pro-OH

HRID 483642

反応式

HRID 483642 の反応式
CN1CCOCC1.[NH:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11].[NH:16]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:17][C:18](ON1C(=O)CCC1=O)=[O:19]>CN(C=O)C>[NH:16]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:17][C:18]([N:8]1[CH2:15][CH2:14][CH2:13][C@H:9]1[C:10]([OH:12])=[O:11])=[O:19]

参加物

5

反応物 3

HCID 79724-Methylmorpholine2 回HCID 76926N-(tert-Butyloxycarbonyl)glycine N-hydroxysuccinimide esterHCID 145742L-Proline

生成物 1

HCID 11673468Boc-gly-pro-OH

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1.4 ml (11 mmol) of N-methylmorpholine are added to 1.15 g (10 mmol) of proline in 50 ml of DMF. The mixture is cooled with an ice bath, 3.06 g (10 mmol) of Boc-Gly-OSu are then added and the pH is adjusted to between 6 and 7 throughout the reaction (14 h) by successive additions of small amounts of N-methylmorpholine (this substance is used as a proton acceptor). The DMF is evaporated off and the evaporation residue is taken up with AcOEt; after precipitation in petroleum ether and then filtration, the expected product is collected.

後処理

  1. temperatureThe mixture is cooled with an ice bath
  2. customThe DMF is evaporated off
  3. customafter precipitation in petroleum ether
  4. filtrationfiltration
  5. customthe expected product is collected

出典と根拠

ORDレコード
ord-46a95c7b3d8442cca33271779bfafde1
出典データセット
uspto-grants-1993_07
特許番号
US05225532

関連ノート

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