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Sodium Carbonate → (S)-2-tert-Butoxycarbonylamino-3-{(S)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl}-propionic acid methyl ester

HRID 39057
ノート
印刷プレビュー

反応式

HRID 39057 の反応式
[CH3:1][O:2][C:3](=[O:24])[C@@H:4]([NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([N+:13]([O-])=O)[CH:7]=1.C[O:26][C:27](=O)[C@@H:28]([C:30]1[CH:35]=[CH:34][C:33]([O:36][CH2:37][C:38]2[CH:43]=[CH:42][C:41]([Cl:44])=[C:40]([Cl:45])[CH:39]=2)=[CH:32][CH:31]=1)O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl.[Fe].CCOC(C)=O>[CH3:1][O:2][C:3](=[O:24])[C@@H:4]([NH:16][C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:5][C:6]1[CH:11]=[CH:10][C:9]2[O:12][C@@H:28]([C:30]3[CH:31]=[CH:32][C:33]([O:36][CH2:37][C:38]4[CH:43]=[CH:42][C:41]([Cl:44])=[C:40]([Cl:45])[CH:39]=4)=[CH:34][CH:35]=3)[C:27](=[O:26])[NH:13][C:8]=2[CH:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 15518593(S)-2-tert-Butoxycarbonylamino-3-(4-hydroxy-3-nitro-phenyl)-propionic acid methyl esterHCID 24965837Methyl (R)-2-(4-((3,4-dichlorobenzyl)oxy)phenyl)-2-hydroxyacetate

生成物 1

HCID 66922588
(S)-2-tert-Butoxycarbonylamino-3-{(S)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl}-propionic acid methyl ester
収率 56.4%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
-20 °C

実験手順

(S)-2-tert-Butoxycarbonylamino-3-(4-hydroxy-3-nitro-phenyl)-propionic acid methyl ester (16.8 mmol) and (R)-[4-(3,4-dichloro-benzyloxy)-phenyl]-hydroxy-acetic acid methyl ester (20.1 mmol) were dissolved in 80 mL of DCM, resin-bound triphenylphosphine (33.6 mmol) added and the mixture cooled to −20° C. To this solution was added DIAD (25.2 mmol) and the mixture was agitated for 30 min at −20° C. The mixture was slowly allowed to warm to r.t. and agiated for 1.5 h. The reaction mixture was filtered and concentrated. The resulting residue was dissolved in glacial acetic acid (60 mL) and heated to 100° C. Iron powder (336 mmol) was added and the resulting mixture heated at 100° C. for 1 h. The mixture was poured onto water and EtOAc. The mixture was brought to ˜pH 7 with sodium carbonate. The organic layer was dried over sodium sulfate and concentrated. The residue was treated with diethyl ether and the resulting solid filtered and washed with diethyl ether to provide (S)-2-tert-Butoxycarbonylamino-3-{(S)-2-[4-(3,4-dichloro-benzyloxy)-phenyl]-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl}-propionic acid methyl ester (5.7 g). LC-MS (m/z) 502 (M-Boc).

後処理

  1. temperatureto warm to r.t.
  2. waitagiated for 1.5 h
  3. filtrationThe reaction mixture was filtered
  4. concentrationconcentrated
  5. dissolutionThe resulting residue was dissolved in glacial acetic acid (60 mL)
  6. temperatureheated to 100° C
  7. temperaturethe resulting mixture heated at 100° C. for 1 h
  8. dry with materialThe organic layer was dried over sodium sulfate
  9. concentrationconcentrated
  10. additionThe residue was treated with diethyl ether
  11. filtrationthe resulting solid filtered
  12. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-982a21edcd44406fbb8fef7df502cbe7
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524708B2

反応ノート

読み込み中…

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