Diethylamine → HCID 21054824、化合物

HRID 2376906

反応式

HRID 2376906 の反応式
[C:1]1([NH:7][C:8]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([NH:19][C:20]4[CH:25]=[CH:24][N:23]=[C:22]([NH2:26])[CH:21]=4)=[CH:16][CH:17]=3)[CH:12]=[CH:11]2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:27]([N:29]([CH2:32][CH3:33])[CH2:30]C)[CH3:28].ClC(OC1C=CC=CC=1)=[O:36].C(NCC)C>O1CCCC1>[C:1]1([NH:7][C:8]([N:10]2[C:18]3[C:13](=[CH:14][C:15]([NH:19][C:20]4[CH:25]=[CH:24][N:23]=[C:22]([NH:26][C:30]([N:29]([CH2:32][CH3:33])[CH2:27][CH3:28])=[O:36])[CH:21]=4)=[CH:16][CH:17]=3)[CH:12]=[CH:11]2)=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 8021DiethylamineHCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 210548085-(2-Aminopyridin-4-ylamino)indole-1-carboxylic acid phenylamide

生成物 1

HCID 21054824HCID 21054824、化合物収率 2.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5-(2-Aminopyridin-4-ylamino)indole-1-carboxylic acid phenylamide (69 mg, 0.20 mmol) was dissolved in tetrahydrofuran (14 ml); triethylamine (0.055 ml, 0.40 mmol) was added thereto; and phenyl chloroformate (0.038 ml, 0.30 mmol) was added thereto while cooling with ice and stirring. A portion of 7.0 ml of the reaction mixture was transferred to another vessel and concentrated under reduced pressure. After the residue was dissolved in N,N-dimethylformamide (1.0 ml), the similar reaction to Example 27 was performed by use of diethylamine (0.031 ml, 0.30 mmol). The obtained crude product was purified by TLC plate (Fuji Silysia NH, developing solvent: ethyl acetate) to yield the title compound (2.0 mg, 0.005 mmol) as pale yellow crystals.

後処理

  1. temperaturewhile cooling with ice
  2. concentrationconcentrated under reduced pressure
  3. dissolutionAfter the residue was dissolved in N,N-dimethylformamide (1.0 ml)
  4. customthe similar reaction to Example 27
  5. customThe obtained crude product
  6. customwas purified by TLC plate (Fuji Silysia NH, developing solvent: ethyl acetate)

出典と根拠

ORDレコード
ord-490c5dd50a4a492fa00688dc098473d1
出典データセット
uspto-grants-2008_12
特許番号
US07468380B2

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