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1,2-Dichloroethane → HCID 68674801、化合物

HRID 1160322
ノート
印刷プレビュー

反応式

HRID 1160322 の反応式
O[N:2]1C2C=CC=CC=2N=N1.C(Cl)CCl.[C:15]([O:19][C:20](=[O:50])[CH2:21][CH:22]([C:26]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][C:34]2[CH:35]=[C:36]([C:40]3[CH:45]=[CH:44][C:43]([C:46]([F:49])([F:48])[F:47])=[CH:42][CH:41]=3)[CH:37]=[CH:38][CH:39]=2)=[CH:28][CH:27]=1)[C:23](O)=[O:24])([CH3:18])([CH3:17])[CH3:16].[OH-].[NH4+]>ClCCl>[C:15]([O:19][C:20](=[O:50])[CH2:21][CH:22]([C:26]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][C:34]2[CH:35]=[C:36]([C:40]3[CH:45]=[CH:44][C:43]([C:46]([F:49])([F:48])[F:47])=[CH:42][CH:41]=3)[CH:37]=[CH:38][CH:39]=2)=[CH:28][CH:27]=1)[C:23]([NH2:2])=[O:24])([CH3:18])([CH3:17])[CH3:16]
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 111,2-DichloroethaneHCID 14923Ammonium HydroxideHCID 757711-HydroxybenzotriazoleHCID 68675946HCID 68675946、化合物

生成物 1

HCID 68674801HCID 68674801、化合物収率 96.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-hydroxybenzotriazole (225 mg, 1.65 mmol) and EDC (315 mg, 1.65 mmol) were added sequentially to compound 50.3 (750 mg, 1.5 mmol) in dichloromethane (25 mL). The resulting mixture was stirred for 1 h before ammonium hydroxide (25% in water, 630 mg, 4.5 mmol) was added dropwise. The reaction was quenched after 30 min. with water (10 mL). The reaction mixture was extracted with dichloromethane (10 mL×3). The organic extracts were combined, dried over MgSO4 and concentrated under reduced pleasure. The product was purified via flash chromatography (50% ethyl acetate in hexanes) to yield 51.1 (720 mg) as a white solid. MS ESI (pos.) m/e: 500 (M+H). 1H NMR (400 MHz) (CDCl3) δ 7.72 (4H, s); 7.68 (1H, s); 7.57-7.48 (3H, m); 7.29-7.25 (2H, m); 7.0-6.97 (2H, d, J=6,8 Hz); 5.14 (2H, s); 3.91-3.88 (1H, m); 3.19-3.13 (1H, m); 2.60-2.55 (1H, m); 1.4 (9H, s).

後処理

  1. additionwas added dropwise
  2. customThe reaction was quenched after 30 min. with water (10 mL)
  3. extractionThe reaction mixture was extracted with dichloromethane (10 mL×3)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pleasure
  6. customThe product was purified via flash chromatography (50% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-a277785666c94d7892e131112cefae0d
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07816367B2

反応ノート

読み込み中…

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