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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → HCID 69676422、化合物

HRID 919616
ノート
印刷プレビュー

反応式

HRID 919616 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][CH2:10][C:11]([OH:13])=O)[CH:5]=[C:6]([Cl:8])[CH:7]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.[CH3:35][CH:36]1[CH2:41][CH2:40][NH:39][CH2:38][CH:37]1[NH:42][C:43](=[O:49])[O:44][C:45]([CH3:48])([CH3:47])[CH3:46].CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:8][C:6]1[CH:5]=[C:4]([NH:9][CH2:10][C:11]([N:39]2[CH2:40][CH2:41][CH:36]([CH3:35])[CH:37]([NH:42][C:43](=[O:49])[O:44][C:45]([CH3:48])([CH3:47])[CH3:46])[CH2:38]2)=[O:13])[CH:3]=[C:2]([Cl:1])[CH:7]=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 5

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 13138167(3,5-Dichlorophenyl)glycineHCID 45092184HCID 45092184、化合物

生成物 1

HCID 69676422HCID 69676422、化合物収率 55.7%

試薬・触媒・溶媒

1
HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-(3,5-dichlorophenylamino)acetic acid (153 mg, 0.69 mmol) in DMF (5 mL) was added HOBt (141 mg, 1.0 mmol), EDCI (201 mg, 1.0 mmol), tert-butyl 4-methylpiperidin-3-ylcarbamate (150 mg, 0.69 mmol), and DIEA (0.18 mL, 1.3 mmol) at 0° C. Then the reaction mixture was stirred at rt for 5 h, partitioned between EtOAc and water. The organic phase was separated and washed with brine, and concentrated in vacuo to yield the crude product, which was purified by column chromatography using 0-2% MeOH: DCM solvent mixture to yield the titled intermediate (160 mg, 54%) as a thick liquid. 1H NMR (400 MHz, CDCl3): δ 6.92 (s, 1H), 6.49 (s, 1H), 6.38 (s, 1H), 6.29 (s, 1H), 5.22-5.15 (m, 1H), 4.65-4.56 (m, 1H), 4.35-4.16 (m, 2H), 3.25-2.89 (m, 2H), 2.85-2.69 (m, 2H), 1.82-1.75 (m, 2H), 1.69-1.45 (m, 1H), 1.22 and 1.14 (2s, 9H), 1.05 and 0.95 (2d, J=6.8 Hz, 3H). LC-MS: m/z [M+1]=416.

後処理

  1. custompartitioned between EtOAc and water
  2. customThe organic phase was separated
  3. washwashed with brine
  4. concentrationconcentrated in vacuo
  5. customto yield the crude product, which
  6. customwas purified by column chromatography

出典と根拠

ORDレコード
ord-06a4be527ef8494bbd61dc68665e11ee
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273028B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート