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2-Chloro-6-fluorobenzoic acid → HCID 178497001、化合物

HRID 1898335
ノート
印刷プレビュー

反応式

HRID 1898335 の反応式
[NH2:1][C:2]1[NH:6][C:5]2[C:7]3[CH2:8][C:9]([CH3:19])([CH3:18])[O:10][C:11]=3[C:12]([C:14]([O:16][CH3:17])=[O:15])=[CH:13][C:4]=2[N:3]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.[Cl:42][C:43]1[CH:51]=[CH:50][CH:49]=[C:48]([F:52])[C:44]=1[C:45](O)=[O:46]>C1COCC1>[Cl:42][C:43]1[CH:51]=[CH:50][CH:49]=[C:48]([F:52])[C:44]=1[C:45]([NH:1][C:2]1[NH:6][C:5]2[C:7]3[CH2:8][C:9]([CH3:19])([CH3:18])[O:10][C:11]=3[C:12]([C:14]([O:16][CH3:17])=[O:15])=[CH:13][C:4]=2[N:3]=1)=[O:46]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 679472-Chloro-6-fluorobenzoic acidHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 178497007HCID 178497007、化合物

生成物 1

HCID 178497001HCID 178497001、化合物収率 44%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of methyl 2-amino-7,7-dimethyl-7,8-dihydro-1H-benzofuro[4,5-d]imidazole-5-carboxylate (1.00 g, 3.81 mmol) in THF (25 mL) was added EDCI.HCl (1.4 g, 7.62 mmol), HOBT (1.00 g, 7.62 mmol), 2-chloro-6-fluorobenzoic acid (1.32 g 7.62 mmol) and TEA (3 mL). The reaction mass was stirred for 18 h. The reaction mass was quenched in water extracted with 10% DCM: methanol. The organic layer was dried over anhydrous sodium sulphate and concentrated. The obtained crude was purified by column chromatography on basic alumina eluting with 0.7% DCM: MeOH to afford 0.700 g of the desired product. 1HNMR (DMSO-d6): δ 1.43 (s, 6H), 3.02 (s, 2H), 3.58 (s, 3H), 6.08 (bs, 1H), 7.59-7.69 (m, 2H), 7.83 (q, J=6.6 Hz, 1H), 8.14 (bs, 2H); MS [M+H]+: 418.05.

後処理

  1. customThe reaction mass was quenched in water
  2. extractionextracted with 10% DCM
  3. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  4. concentrationconcentrated
  5. customThe obtained crude
  6. customwas purified by column chromatography on basic alumina eluting with 0.7% DCM

出典と根拠

ORDレコード
ord-022176e27aff4db89bc1ac7ca7883710
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08519149B2

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