Acetic Anhydride → HCID 18432836、化合物

HRID 1108226ノート

反応式

HRID 1108226 の反応式
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].C(OC(=O)C)(=O)C.[Cl:14][C:15]1[CH:25]=[CH:24][C:18]([CH2:19][NH:20][C:21]([NH2:23])=[O:22])=[CH:17][CH:16]=1>C1(C)C=CC=CC=1>[Cl:14][C:15]1[CH:25]=[CH:24][C:18]([CH2:19][NH:20][C:21]([NH:23][C:4](=[O:6])[CH2:3][C:1]#[N:2])=[O:22])=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 7918Acetic Anhydride2 回HCID 9740Cyanoacetic acidHCID 1484508N-(4-chlorobenzyl)urea

生成物 1

HCID 18432836HCID 18432836、化合物収率 85.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

68.7 g of 98% cyanoacetic acid and 155 ml of acetic anhydride were kept at 65° C. for 30 minutes. 4-chlorobenzylurea (132.9 g) was added in portions over 10 minutes. After 2 hrs. at 70-75° C., further acetic anhydride (25 ml) was added. After a further 15 minutes, 90 ml of toluene was added, cooled to room temperature, the solid collected and washed with toluene to give the title compound (155.60 g) as a white solid mp 203-6° C.

後処理

  1. waitAfter a further 15 minutes
  2. customthe solid collected
  3. washwashed with toluene

出典と根拠

ORDレコード
ord-d50de089d4664613b4d24a67a86b2f83
出典データセット
uspto-grants-2000_05
特許番号
US06066641

反応ノート

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