Iodoacetamide → HCID 44415988、化合物

HRID 1289945ノート

反応式

HRID 1289945 の反応式
[F:1][C:2]([F:29])([F:28])[C:3]1[CH:4]=[C:5]([CH2:13][O:14][CH:15]2[CH2:19][CH2:18][CH:17]([NH:20][CH3:21])[CH:16]2[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.I[CH2:31][C:32]([NH2:34])=[O:33].CCN(C(C)C)C(C)C>C(#N)C>[F:1][C:2]([F:28])([F:29])[C:3]1[CH:4]=[C:5]([CH2:13][O:14][CH:15]2[CH2:19][CH2:18][CH:17]([N:20]([CH2:31][C:32]([NH2:34])=[O:33])[CH3:21])[CH:16]2[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1

参加物

5

反応物 3

HCID 3727IodoacetamideHCID 81531DiisopropylethylamineHCID 75024269HCID 75024269、化合物

生成物 1

HCID 44415988HCID 44415988、化合物収率 123.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A solution of 50 mg of amine prepared in Example 11, 33 mg of iodoacetamide and 0.05 mL of DIPEA in 0.5 mL of acetonitrile was heated in a sealed vial at 50° C. for 2 h (or room temperature for 16 h). The volatiles were evaporated under a stream of nitrogen and the residue was purified on a 1 mm preparative silica gel plate eluted with 5% MeOH in methylene chloride to afford 70 mg of title compound. Mass spec (NH3 /CI): 475 (M+1).

後処理

  1. customThe volatiles were evaporated under a stream of nitrogen
  2. customthe residue was purified on a 1 mm preparative silica gel plate
  3. washeluted with 5% MeOH in methylene chloride

出典と根拠

ORDレコード
ord-312fc7ca520c4272950303a67197ca16
出典データセット
uspto-grants-1998_05
特許番号
US05750549

反応ノート

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