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Benzyloxycarbonyl-L-methionine → 2-(morpholinomethyl)prop-2-yl (2S)-2-(benzyloxycarbonylamino)-4-methylsulfanylbutyrate

HRID 1251879
ノート
印刷プレビュー

反応式

HRID 1251879 の反応式
[OH:1][C:2]([CH3:11])([CH3:10])[CH2:3][N:4]1[CH2:9][CH2:8][O:7][CH2:6][CH2:5]1.[CH2:12]([O:19][C:20]([NH:22][C@H:23]([C:28](O)=[O:29])[CH2:24][CH2:25][S:26][CH3:27])=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.F[P-](F)(F)(F)(F)F.Br[P+](N1CCCC1)(N1CCCC1)N1CCCC1>CN(C1C=CN=CC=1)C.ClCCl>[CH2:12]([O:19][C:20]([NH:22][C@@H:23]([CH2:24][CH2:25][S:26][CH3:27])[C:28]([O:1][C:2]([CH2:3][N:4]1[CH2:5][CH2:6][O:7][CH2:8][CH2:9]1)([CH3:11])[CH3:10])=[O:29])=[O:21])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=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 3

HCID 1550857Benzyloxycarbonyl-L-methionineHCID 2733179PyBroPHCID 222731702-Methyl-1-morpholinopropan-2-ol

生成物 1

HCID 865851352-(morpholinomethyl)prop-2-yl (2S)-2-(benzyloxycarbonylamino)-4-methylsulfanylbutyrate収率 40%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒

実験手順

A solution of N-(2-hydroxy-2-methylpropyl)morpholine (9.8 g, 62 mmol), N-benzyloxycarbonyl-L-methionine (12.6 g, 44 mmol), bromo-tris-pyrrolidino-phosphonium hexafluorophosphate (25 g, 54 mmol), DMAP (5.4 g, 44 mmole) in dichloromethane (250 ml) was stirred, in the presence of 4 Å molecular sieves (5 g), at ambient temperature for 48 h. After evaporation to dryness, the mixture was taken up in diethyl ether and the insoluble material eliminated by filtration. The organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and a saturated solution of brine, evaporated to dryness and purified by flash column chromatography eluting with dichloromethane/ethanol (98:2) to give 2-(morpholinomethyl)prop-2-yl (2S)-2-(benzyloxycarbonylamino)-4-methylsulfanylbutyrate (40%).

後処理

  1. customAfter evaporation to dryness
  2. filtrationthe insoluble material eliminated by filtration
  3. washThe organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate
  4. customa saturated solution of brine, evaporated to dryness
  5. custompurified by flash column chromatography
  6. washeluting with dichloromethane/ethanol (98:2)

出典と根拠

ORDレコード
ord-fb2d2d95a9cc4d629489a2b647bfd7b1
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06342765B1

反応ノート

読み込み中…

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