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1-Hydroxybenzotriazole → HCID 18976209、化合物

HRID 2393590
ノート
印刷プレビュー

反応式

HRID 2393590 の反応式
Cl.CN(C)CCCN=C=NCC.Cl.[NH2:14][CH:15]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[N:17]([CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:16]1=[O:29].[CH2:30]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH2:33][CH2:32][CH:31]1[C:40](O)=[O:41].ON1C2C=CC=CC=2N=N1>C(N(CC)CC)C.C(Cl)Cl>[O:29]=[C:16]1[CH:15]([NH:14][C:40]([CH:31]2[CH2:32][CH2:33][C:34]3[C:39](=[CH:38][CH:37]=[CH:36][CH:35]=3)[CH2:30]2)=[O:41])[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[N:17]1[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 1013701,2,3,4-Tetrahydro-2-naphthoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 18976150HCID 18976150、化合物

生成物 1

HCID 18976209HCID 18976209、化合物収率 75.4%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8471Triethylamine溶媒

実験手順

Under ice cooling, 1.10 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride was added to a stirred mixture of 1.22 g of 3-amino-2,3-dihydro-1-pentyl-1H-indol-2-one hydrochloride, 0.93 g of 1,2,3,4-tetrahydronaphthalene-2-carboxylic acid, 0.72 g of 1-hydroxybenzotriazole and 40 ml of methylene chloride. After the reaction mixture was stirred under ice cooling for 1 hour, 1.0 ml of triethylamine was added to the mixture. The resulting mixture was stirred under ice cooling for 2 hours and then stirred at room temperature for 2 hours. The solvent was removed by evaporation under reduced pressure. The residue was extracted with ethyl acetate, and the extract was washed and dried. After removal of solvent, the residual solid was recrystallized from ethyl acetate-hexane to afford 1.36 g of N-(2,3-dihydro-2-oxo-1-pentyl-1H-indol-3-yl)-1,2,3,4-tetrahydronaphthalene-2-carboxamide as colorless crystals. Melting point: 127° to 132° C., IR (Nujol) (cm-1): 3280, 1725, 1640, 1610, MS (m/z): 376 (M+), 218 (base), 147, 31.

後処理

  1. stirringThe resulting mixture was stirred under ice cooling for 2 hours
  2. stirringstirred at room temperature for 2 hours
  3. customThe solvent was removed by evaporation under reduced pressure
  4. extractionThe residue was extracted with ethyl acetate
  5. washthe extract was washed
  6. customdried
  7. customAfter removal of solvent
  8. customthe residual solid was recrystallized from ethyl acetate-hexane

出典と根拠

ORDレコード
ord-57c7ca4161c945328ec46f4abe9b3bf8
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05807883

反応ノート

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