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4-Nitrobenzoic Acid → 4-nitrobenzoic acid (S)-1-[(3R,5R)-5-(4-chlorophenyl)morpholin-3-yl]ethyl ester

HRID 1677065
ノート
印刷プレビュー

反応式

HRID 1677065 の反応式
CC(OC(/N=N/C(OC(C)C)=O)=O)C.[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([C@H:22]2[NH:27][C@@H:26]([C@H:28]([OH:30])[CH3:29])[CH2:25][O:24][CH2:23]2)=[CH:18][CH:17]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N+:50]([C:53]1[CH:61]=[CH:60][C:56]([C:57](O)=[O:58])=[CH:55][CH:54]=1)([O-:52])=[O:51]>C(OCC)(=O)C.O.O1CCCC1>[Cl:15][C:16]1[CH:17]=[CH:18][C:19]([C@H:22]2[NH:27][C@@H:26]([C@@H:28]([O:30][C:57](=[O:58])[C:56]3[CH:55]=[CH:54][C:53]([N+:50]([O-:52])=[O:51])=[CH:61][CH:60]=3)[CH3:29])[CH2:25][O:24][CH2:23]2)=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 61084-Nitrobenzoic AcidHCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 67371750(R)-1-[(3R,5R)-5-(4-chlorophenyl)morpholin-3-yl]ethanol

生成物 1

HCID 673717534-nitrobenzoic acid (S)-1-[(3R,5R)-5-(4-chlorophenyl)morpholin-3-yl]ethyl ester収率 100%

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Under a nitrogen atmosphere and under ice-cooling, diisopropylazodicarboxylate (1.36 mL) was added dropwise in a tetrahydrofuran solution containing (R)-1-[(3R,5R)-5-(4-chlorophenyl)morpholin-3-yl]ethanol (903 mg), triphenylphosphine (1.81 g), and 4-nitrobenzoic acid (1.16 g). Stirring was continued for 30 minutes at the same temperature and for 2 hours at room temperature. Water and ethyl acetate was added to the reaction solution, and the organic layer was partitioned. The organic layer was washed with brine and was dried over anhydrous magnesium sulfate. The solvent was removed under a vacuum, and the residue was purified by silica gel column chromatography (heptane/ethyl acetate 9/1→8/2→7/3), and the title compound (1.46 g) was obtained. The physical property values are as follows.

後処理

  1. temperatureUnder a nitrogen atmosphere and under ice-cooling
  2. customthe organic layer was partitioned
  3. washThe organic layer was washed with brine
  4. dry with materialwas dried over anhydrous magnesium sulfate
  5. customThe solvent was removed under a vacuum
  6. customthe residue was purified by silica gel column chromatography (heptane/ethyl acetate 9/1→8/2→7/3)

出典と根拠

ORDレコード
ord-aeb90c0291514159983613fdf2b4b66c
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08008293B2

反応ノート

読み込み中…

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