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Cyclohexylamine → HCID 136169029、化合物

HRID 68938
ノート
印刷プレビュー

反応式

HRID 68938 の反応式
[OH:1][C:2]1[N:3]=[C:4]2[S:13][C:12]3[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[N:5]2[C:14](=[O:23])[C:15]=1[C:16]([NH:18][CH2:19][C:20]([OH:22])=O)=[O:17].C(N(CC)CC)C.[CH:31]1([NH2:37])[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1.OC1C2N=NNC=2C=CC=1.Cl.CN(C)CCCN=C=NCC>ClCCl.CO>[CH:31]1([NH:37][C:20]([CH2:19][NH:18][C:16]([C:15]2[C:14](=[O:23])[N:5]3[C:6]4[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]=4[S:13][C:4]3=[N:3][C:2]=2[OH:1])=[O:17])=[O:22])[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 7965CyclohexylamineHCID 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 136008904Glycine, N-[(7,8,9,10-tetrahydro-2-hydroxy-4-oxo-4H,6H-cyclohepta[4,5]thiazolo[3,2-a]pyrimidin-3-yl)carbonyl]-HCID 178418300HCID 178418300、化合物

生成物 1

HCID 136169029
HCID 136169029、化合物
収率 71.7%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

実験手順

To the stirred suspension of [(2-hydroxy-4-oxo-6,7,8,9-tetrahydro-4H,5H-10-thia-1,4a-diaza-benzo[a]azulene-3-carbonyl)-amino]-acetic acid (0.70 gm, 0.0020 mole) in dichloromethane (20 ml), triethylamine (0.85 ml, 0.0062 mole) and cyclohexylamine (0.29 ml, 0.0025 mole) were added. To the reaction mixture, hydroxybenzotriazole (0.28 gm, 0.0020 mole) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.60 gm, 0.0031 mole) were added and stirred at room temperature for 12 hrs. Dichloromethane was distilled off and 1N hydrochloric acid (50 ml) was added to the residue, the separated solid was collected by filtration. The solid thus obtained was stirred in methanol (20 ml) at 60° C. for 0.5 hr, filtered and suck dried to give 0.60 gm title compound.

後処理

  1. additionwere added
  2. distillationDichloromethane was distilled off
  3. addition1N hydrochloric acid (50 ml) was added to the residue
  4. filtrationthe separated solid was collected by filtration
  5. customThe solid thus obtained
  6. filtrationfiltered
  7. customsuck dried

出典と根拠

ORDレコード
ord-ef3a88a3976a4fefb464a042ee6851af
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08822484B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート