O-Phenylenediamine → HCID 44540253、化合物

HRID 1926201ノート

反応式

HRID 1926201 の反応式
[CH3:1][O:2][C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([O:16][CH3:17])=[CH:10][CH:11]=3)[C:6](=[CH:18][C:19]([NH:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27](O)=[O:28])=[O:20])[C:5]=2[CH:4]=1.Cl.C(N=C=NCCCN(C)C)C.O[C:43]1[C:51]2[N:50]=N[NH:48][C:47]=2[CH:46]=[CH:45][CH:44]=1.C(N(CC)CC)C.C1(N)C=CC=CC=1N>[Cl-].[Na+].O.CN(C=O)C>[CH3:1][O:2][C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][C:9]([O:16][CH3:17])=[CH:10][CH:11]=3)[C:6](=[CH:18][C:19]([NH:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][C:27]([NH:48][C:47]3[CH:46]=[CH:45][CH:44]=[CH:43][C:51]=3[NH2:50])=[O:28])=[O:20])[C:5]=2[CH:4]=1

参加物

8

反応物 5

HCID 7243O-PhenylenediamineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 67520974HCID 67520974、化合物HCID 178418300HCID 178418300、化合物

生成物 1

HCID 44540253HCID 44540253、化合物収率 77%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

6-(2-(2,7-dimethoxy-9H-fluoren-9-ylidene)acetamido)hexanoic acid (395 mg, 1 mmol), and 8 ml of DMF were stirred at room temperature while 1-Ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (394 mg, 2 mmol), hydroxy-benzotriazole (162 mg, 1.2 mmol), triethylamine (404 mg, 4 mmol) and o-phenylenediamine (432 mg, 4 mmol) were added. The mixture was stirred for 24 hours at room temperature. The mixture was diluted with 400 mL of brine. The solids were collected by vacuum filtration, washed with water and dried under vacuum to give the title compound (373 mg, 77% yield) as a brown solid. LC-MS (m/z) 486 (M+1).

後処理

  1. additionwere added
  2. filtrationThe solids were collected by vacuum filtration
  3. washwashed with water
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-60df78d54c91496ea6eb4453456fa256
出典データセット
uspto-grants-2012_05
特許番号
US08178577B2

反応ノート

読み込み中…