Triethylamine → 5-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester

HRID 1926186ノート

反応式

HRID 1926186 の反応式
[CH:1]1[C:13]2[C:12](=[CH:14][C:15](O)=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.C(N=C=NCCCN(C)C)C.OC1C2N=NNC=2C=CC=1.C(N(CC)CC)C.Cl.[CH3:48][O:49][C:50](=[O:56])[CH2:51][CH2:52][CH2:53][CH2:54][NH2:55]>[Cl-].[Na+].O.CN(C=O)C>[CH3:48][O:49][C:50](=[O:56])[CH2:51][CH2:52][CH2:53][CH2:54][NH:55][C:15](=[O:16])[CH:14]=[C:12]1[C:13]2[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=2[C:6]2[C:11]1=[CH:10][CH:9]=[CH:8][CH:7]=2

参加物

8

反応物 5

HCID 8471TriethylamineHCID 967929H-Fluoren-9-ylideneacetic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 13672034Methyl 5-aminopentanoate hydrochlorideHCID 178418300HCID 178418300、化合物

生成物 1

HCID 579720535-(2-(9H-fluoren-9-ylidene)acetamido)pentanoic acid methyl ester収率 82.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

2-(9H-fluoren-9-ylidene)acetic acid (222 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), hydroxybenzo-triazole (162 mg, 1.2 mmol), triethylamine (404 mg, 4 mmol) and 5-aminovaleric acid methyl ester hydrochloride (202 mg, 1.2 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 (278 mg, 68% yield) as a white solid. LC-MS (m/z) 336 (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-a479601e4d144f0a8d5655deb5928ce7
出典データセット
uspto-grants-2012_05
特許番号
US08178577B2

反応ノート

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