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Dimethylformamide → tert-butyl (6R,7R)-7-[[(2Z)-2-methoxyimino-2-[2-(tritylamino)-1,3-thiazol-4-yl]acetyl]amino]-3-(oxan-2-yl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate

HRID 612281
ノート
印刷プレビュー

反応式

HRID 612281 の反応式
S(Cl)(C)(=O)=O.Cl.CO[CH:9]([C:13]1[N:14]=[C:15]([NH:19][C:20]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[S:16](=N)[CH:17]=1)[C:10]([OH:12])=O.C([N:42](CC)C(C)C)(C)C.[NH2:48][C@@H:49]1[C:69](=[O:70])[N:51]2[C:52]([C:62]([O:64][C:65]([CH3:68])([CH3:67])[CH3:66])=[O:63])=[C:53]([CH:56]3[CH2:61][CH2:60][CH2:59][CH2:58][O:57]3)[CH2:54][S:55][C@H:50]12.CN([CH:74]=[O:75])C>N1C=CC=CC=1>[CH3:74][O:75]/[N:42]=[C:9](/[C:13]1[N:14]=[C:15]([NH:19][C:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[S:16][CH:17]=1)\[C:10]([NH:48][C@@H:49]1[C:69](=[O:70])[N:51]2[C:52]([C:62]([O:64][C:65]([CH3:67])([CH3:66])[CH3:68])=[O:63])=[C:53]([CH:56]3[CH2:61][CH2:60][CH2:59][CH2:58][O:57]3)[CH2:54][S:55][C@H:50]12)=[O:12]
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

7

反応物 5

HCID 6228Dimethylformamide2 回HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 53828043t-butyl (6R,7R)-7amino-3-(tetrahydropyran-2-yl)-ceph-3-em-4-carboxylateHCID 178478975HCID 178478975、化合物

生成物 1

HCID 141582271
tert-butyl (6R,7R)-7-[[(2Z)-2-methoxyimino-2-[2-(tritylamino)-1,3-thiazol-4-yl]acetyl]amino]-3-(oxan-2-yl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate
収率 62%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
-50 °C

実験手順

Mesyl chloride (121 mg, 82 μl) was added to 2-(Z)-methoxy-imino-2-(2-tritylaminothiazol-4-yl)acetic acid hydrochloride (466 mg) and N,N-diisopropylethylamine (252 mg, 340 μl) in dry DMF (10 ml) at -50° C. under argon and stirred at -50° C. for 1 h. Then t-butyl (6R,7R)-7amino-3- (tetrahydropyran-2-yl)-ceph-3-em-4-carboxylate (Isomer A, 300 mg) in dry DMF (5 ml) followed by pyridine (70 mg, 72 μl) were added and reaction mixture left for a further 1 h whilst warming to ambient temperature. The reaction mixture was partitioned between ethyl acetate and water, reextracted with ethyl acetate, organic extracts washed with water (x3) and brine, dried, concentrated and flash chromatography (eluting with 30, 40, 50, 60% ethyl acetate in hexane) to afford the title compound as a pale yellow foam (420 mg, 62%); νmax (CH2Cl2) 3420, 1784, 1732 (shoulder), 1717, 1685 cm-1 ; δH (CDCl3), 1.53 (9 H, s) overlapping 1.4-1.7 (4 H, m), 1.73-1.94 (2 H, m), 3.38-3.58 (3 H, m), 3.95-4.00 (1 H, m), 4.07 (3 H, s), 4.54-4.59 (1 H, m), 5.02 (1 H, d, J4.8 Hz), 5.90 (1 H, dd, J4.5, 9.1 Hz) 6.74 (1 H, s), 6.86 (1 H, d, J8.8 Hz), 7.04 (1 H, s) and 7.30 (15 H, s). [Mass spectrum: +ve ion (3-nitrobenzyl alcohol, sodium acetate) MNa+ (788)].

後処理

  1. additionwere added
  2. customreaction mixture
  3. waitleft for a further 1 h
  4. temperaturewhilst warming to ambient temperature
  5. customThe reaction mixture was partitioned between ethyl acetate and water
  6. washwashed with water (x3) and brine
  7. customdried
  8. concentrationconcentrated
  9. washflash chromatography (eluting with 30, 40, 50, 60% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-8bf52f8d39574935a3d4a403a78b4e30
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06001997

反応ノート

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