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HCID 69083734、化合物 → HCID 69280781、化合物

HRID 1396248
ノート
印刷プレビュー

反応式

HRID 1396248 の反応式
[Li][CH2:2]CCC.[CH:6]([C@H:8]1[O:16][C@H:15]2[C@H:11]([N:12]=[C:13]([N:17]([CH3:25])[C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[S:14]2)[C@@H:10]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=2)[C@@H:9]1[O:36][CH2:37][C:38]1[CH:43]=[CH:42][C:41]([O:44][CH3:45])=[CH:40][CH:39]=1)=O.OC[C@H]1O[C@H]2[C@H](N=C(N(C)C(=O)OC(C)(C)C)S2)[C@@H](OCC2C=CC(OC)=CC=2)[C@@H]1OCC1C=CC(OC)=CC=1.CN(C)C1S[C@H]2O[C@H](CO)[C@@H](OCC3C=CC(OC)=CC=3)[C@H](OCC3C=CC(OC)=CC=3)[C@H]2N=1>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O1CCCC1>[CH3:45][O:44][C:41]1[CH:42]=[CH:43][C:38]([CH2:37][O:36][C@@H:9]2[C@@H:8]([CH:6]=[CH2:2])[O:16][C@H:15]3[C@H:11]([N:12]=[C:13]([N:17]([CH3:25])[C:18](=[O:24])[O:19][C:20]([CH3:21])([CH3:22])[CH3:23])[S:14]3)[C@H:10]2[O:26][CH2:27][C:28]2[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=2)=[CH:39][CH:40]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 69083734HCID 69083734、化合物HCID 69280765HCID 69280765、化合物HCID 86701105HCID 86701105、化合物HCID 178418339Butyllithium

生成物 1

HCID 69280781HCID 69280781、化合物

試薬・触媒・溶媒 2

HCID 74505
Methyltriphenyliphosphonium bromide
触媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of methyltriphenylphosphonium bromide (1.85 g, 5.18 mmol) in tetrahydrofuran (35 mL) was treated with n-BuLi (1.9 ml, 2.5M) for 30 min at 0° C., and followed by addition of tert-butyl (3aR,5S,6S,7R,7aR)-5-formyl-6,7-bis(4-methoxybenzyloxy)-5,6,7,7a-tetrahydro-3aH-pyrano[3,2-d]thiazol-2-yl(methyl)carbamate (44) prepared from compound 28 by a procedure identical to that described for the conversion of 10 to 11) (0.6 g, 1.05 mmol) in THF (5 mL). The resulting solution was stirred overnight at room temperature, quenched by water (25 mL), and extracted with dichloromethane (3×25 ml). The combined organic layers were dried over magnesium sulfate and concentrated under vacuum to give a residue, which was purified by a silica gel column, eluted with 20% ethyl acetate in petroleum ether to give crude compound 45 as a yellow oil (220 mg, purity 50% by LC-MS). (ES, m/z): [M+H]+ 571.0.

後処理

  1. customquenched by water (25 mL)
  2. extractionextracted with dichloromethane (3×25 ml)
  3. dry with materialThe combined organic layers were dried over magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. customto give a residue, which
  6. customwas purified by a silica gel column
  7. washeluted with 20% ethyl acetate in petroleum ether

出典と根拠

ORDレコード
ord-2edf49bb4f0344a48b514003264fa21d
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901087B2

反応ノート

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