ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1-Hydroxybenzotriazole → HCID 66864043、化合物

HRID 2093430
ノート
印刷プレビュー

反応式

HRID 2093430 の反応式
ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([C:49]2[CH:54]=[CH:53][C:52]([Cl:55])=[CH:51][CH:50]=2)[N:31]2[CH2:34][CH:33]([CH2:35][S:36]([NH:39][C:40]3[CH:41]=[C:42]([CH:46]=[CH:47][CH:48]=3)[C:43]([OH:45])=O)(=[O:38])=[O:37])[CH2:32]2)=[CH:26][CH:25]=1.Cl.[NH2:57][CH2:58][C:59]([N:61]1[CH2:66][CH2:65][O:64][CH2:63][CH2:62]1)=[O:60]>O1CCCC1.ClCCl.C(N(CC)CC)C>[Cl:23][C:24]1[CH:25]=[CH:26][C:27]([CH:30]([C:49]2[CH:54]=[CH:53][C:52]([Cl:55])=[CH:51][CH:50]=2)[N:31]2[CH2:34][CH:33]([CH2:35][S:36]([NH:39][C:40]3[CH:41]=[C:42]([CH:46]=[CH:47][CH:48]=3)[C:43]([NH:57][CH2:58][C:59]([N:61]3[CH2:66][CH2:65][O:64][CH2:63][CH2:62]3)=[O:60])=[O:45])(=[O:37])=[O:38])[CH2:32]2)=[CH:28][CH:29]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 122918142-Amino-1-(morpholin-4-yl)ethan-1-one--hydrogen chloride (1/1)HCID 66864534HCID 66864534、化合物

生成物 1

HCID 66864043HCID 66864043、化合物

試薬・触媒・溶媒 3

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 8471Triethylamine溶媒

反応条件

温度
20 °C

実験手順

67 mg of 1-hydroxybenzotriazole, 0.14 cm3 of triethylamine and 270 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride are added successively to a solution of 500 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)benzoic acid and 215 mg of 2-amino-1-morpholin-4-ylethanone hydrochloride in 15 cm3 of tetrahydrofuran. The reaction mixture is left stirring overnight at a temperature in the region of 20° C. After concentration of the reaction medium to dryness under reduced pressure, the residue obtained is taken up with dichloromethane. The organic phase is washed with water, dried, and concentrated to dryness under reduced pressure, to give a reaction crude which is purified by flash chromatography on a Merck 30 g silica cartridge (elution gradient: 100/0 to 95/5 dichloromethane/methanol). After concentration of the fractions under reduced pressure, a white foam is obtained which crystallizes after trituration with diethyl ether. After filtration and drying using a vane pump, 470 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)-N-(2-morpholin-4-yl-2-oxoethyl)benzamide are thus obtained in the form of white crystals.

後処理

  1. waitThe reaction mixture is left
  2. customAfter concentration of the reaction medium to dryness under reduced pressure, the residue obtained
  3. washThe organic phase is washed with water
  4. customdried
  5. concentrationconcentrated to dryness under reduced pressure
  6. customto give
  7. customa reaction crude which
  8. customis purified by flash chromatography on a Merck 30 g silica cartridge (elution gradient: 100/0 to 95/5 dichloromethane/methanol)
  9. customAfter concentration of the fractions under reduced pressure, a white foam is obtained which
  10. customcrystallizes after trituration with diethyl ether
  11. filtrationAfter filtration
  12. customdrying
  13. customare thus obtained in the form of white crystals

出典と根拠

ORDレコード
ord-9b24d917cc614ef9928ca4e68d8cf6f7
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445478B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート