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Trimethyl phosphonoacetate → HCID 69858985、化合物

HRID 1860294
ノート
印刷プレビュー

反応式

HRID 1860294 の反応式
[CH3:1][O:2][C:3]([CH2:5]P(OC)(OC)=O)=[O:4].C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[CH:22]([C:24]1[CH:29]=[CH:28][C:27](/[C:30](/[C:40]2[CH:45]=[CH:44][C:43]([F:46])=[CH:42][CH:41]=2)=[C:31](\[C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)/[CH2:32][CH3:33])=[CH:26][CH:25]=1)=O>C1COCC1.[Cl-].[Na+].O>[F:46][C:43]1[CH:42]=[CH:41][C:40]([C:30]([C:27]2[CH:26]=[CH:25][C:24]([CH:22]=[CH:5][C:3]([O:2][CH3:1])=[O:4])=[CH:29][CH:28]=2)=[C:31]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH2:32][CH3:33])=[CH:45][CH:44]=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

6

反応物 3

HCID 80029Trimethyl phosphonoacetateHCID 2724254Sodium bis(trimethylsilyl)amideHCID 12085902HCID 12085902、化合物

生成物 1

HCID 69858985HCID 69858985、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒3 回
HCID 57417360
Sodium chloride; water
溶媒

反応条件

温度
-78 °C

実験手順

To a solution of trimethyl phosphonoacetate (412 mg, 2.26 mmol) in THF (15 mL) at 0° C. was added 1M sodium bis(trimethylsilyl)amide in THF (2.26 mL, 2.26 mmol) dropwise. After stirring 15 min the mixture was cooled to −78° C. and a solution of aldehyde (4) (625 mg, 1.89 mmol) in THF (8 mL) was added dropwise. The solution was allowed to warm to rt. After stirring 4 h, brine was added and the mixture was extracted with EtOAc. The combined organic layers were washed with water, brine, and dried (MgSO4). The solvent was removed under reduced pressure and the residue was chromatographed (silica gel, 7.5 to 15% EtOAc/hexanes) to give the ester (5) as a white solid (658 mg, 90%): 1 H NMR (CDCl3) δ 7.52 (d, J=16.1 Hz, 1 H), 7.15 (m, 11 H), 6.86 (d, J=8.1 Hz, 2 H), 6.28 (d, J=16.1 Hz, 1 H), 3.76 (s, 3 H), 2.47 (q, J=7.7 Hz, 2 H), 0.93 (t, J=7.7 Hz, 3 H); APcI m/z: 428 (M+H+CH3CN+, 100%).

後処理

  1. temperatureto warm to rt
  2. stirringAfter stirring 4 h
  3. extractionthe mixture was extracted with EtOAc
  4. washThe combined organic layers were washed with water, brine
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was chromatographed (silica gel, 7.5 to 15% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-9886edc9a2ef4d41a662626952c86ab6
出典データセット
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06528681B2

反応ノート

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