Water → 1-Benzoyl-3-[1-(2-[1,4-benzodioxan-2-yl]-2-oxoethyl)piperid-4-yl]-urea

HRID 225143ノート

反応式

HRID 225143 の反応式
[C:1]([NH:9][C:10]([NH:12][CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1)=[O:11])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:20][C:21]([CH:23]1[O:28][C:27]2[CH:29]=[CH:30][CH:31]=[CH:32][C:26]=2[O:25][CH2:24]1)=[O:22].C(N(CC)CC)C.O>CN(C)C=O>[C:1]([NH:9][C:10]([NH:12][CH:13]1[CH2:18][CH2:17][N:16]([CH2:20][C:21]([CH:23]2[O:28][C:27]3[CH:29]=[CH:30][CH:31]=[CH:32][C:26]=3[O:25][CH2:24]2)=[O:22])[CH2:15][CH2:14]1)=[O:11])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 126085824-BenzoylureidopiperidineHCID 126085852-Bromo-1-(2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-one

生成物 1

HCID 126085861-Benzoyl-3-[1-(2-[1,4-benzodioxan-2-yl]-2-oxoethyl)piperid-4-yl]-urea収率 76%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-Benzoyl-3-(piperid-4-yl)urea (2.46 g, 0.01 mol) and 2-bromoacetyl-1,4-benzodioxan (2.57 g, 0.01 mol) in dry dimethylformamide (40 mls) were stirred at room temperature. Triethylamine (1,1 g, 1.5 cm3) was added and the suspension stirred for 1 hour. Water was added and the solid filtered off (4.20 g, 100%). The solid was suspended in methanol (40 mls) and ethanolic hydrogen chloride added until the solution was acidic. The title compound was filtered off as the hydrochloride salt and dried (yield 3.51 gm 76% yield). Melting pt. 160°-161° C.

後処理

  1. filtrationthe solid filtered off (4.20 g, 100%)
  2. additionethanolic hydrogen chloride added until the solution
  3. filtrationThe title compound was filtered off as the hydrochloride salt
  4. customdried (yield 3.51 gm 76% yield)

出典と根拠

ORDレコード
ord-7223e09ddead4acba80c669284a9b226
出典データセット
uspto-grants-1980_11
特許番号
US04235915

反応ノート

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