Triethylamine → HCID 69453076、化合物

HRID 1517633ノート

反応式

HRID 1517633 の反応式
[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C@H:10]([NH:14][C:15]([NH:17][C:18]1[CH:26]=[CH:25][CH:24]=[C:23]3[C:19]=1[CH:20]=[N:21][N:22]3[C:27]([O:29][CH2:30][P:31](=[O:34])([OH:33])[OH:32])=[O:28])=[O:16])[CH2:9][CH2:8]2)([CH3:4])([CH3:3])[CH3:2].[CH2:35]([N:37]([CH2:40][CH3:41])[CH2:38][CH3:39])[CH3:36]>CO>[CH2:35]([N:37]([CH2:40][CH3:41])[CH2:38][CH3:39])[CH3:36].[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C@H:10]([NH:14][C:15]([NH:17][C:18]1[CH:26]=[CH:25][CH:24]=[C:23]3[C:19]=1[CH:20]=[N:21][N:22]3[C:27]([O:29][CH2:30][P:31](=[O:32])([OH:34])[OH:33])=[O:28])=[O:16])[CH2:9][CH2:8]2)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 8471TriethylamineHCID 16226508HCID 16226508、化合物

生成物 1

HCID 69453076HCID 69453076、化合物収率 100.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Suspended 50.2 mg (103 μmol) of compound from Example 21D in 10 mL methanol, added 10.4 mg (103 μmol) triethylamine, stirred the colorless solution for 10 minutes at ambient temperature, concentrated and vacuum dried. Obtained 61 mg (100% yield) of the title compound as an off-white powder. 1H NMR (methanol-d4) δ: 1.29 (t, 9H), 1.32 (s, 9H), 1.90 (m, 1H), 2.59 (m, 1H), 2.89 (m, 1H), 3.00 (m, 1H), 3.16 (q, 6H), 4.54 (d, 2H), 5.29 (t, 1H), 7.28 (s, 2H), 7.31 (s, 1H), 7.52 (t, 1H), 7.74 (d, 1H), 7.97 (d, 1H), 8.36 (s, 1H). Anal Calcd for C23H27N4O6P.1.0 triethylamine.0.7 methanol: C, 58.47; H, 7.40; N, 11.48. Found: C, 58.46; H, 7.38; N, 11.44.

後処理

  1. concentrationconcentrated
  2. customvacuum dried

出典と根拠

ORDレコード
ord-97fafbc949604f82bbb64d782a995058
出典データセット
uspto-grants-2012_07
特許番号
US08232309B2

反応ノート

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