Tert-butyl N-[(4-cyanophenyl)methyl]-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamate → 4-(Aminomethyl)benzonitrile hydrochloride

HRID 432676

反応式

HRID 432676 の反応式
C(OC([N:8]([CH2:16][C:17]1[CH:24]=[CH:23][C:20]([C:21]#[N:22])=[CH:19][CH:18]=1)C(OC(C)(C)C)=O)=O)(C)(C)C.O1CCOCC1.[ClH:31]>>[ClH:31].[C:16]([C:17]1[CH:24]=[CH:23][C:20]([CH2:21][NH2:22])=[CH:19][CH:18]=1)#[N:8]

参加物

3

反応物 2

HCID 3683768Tert-butyl N-[(4-cyanophenyl)methyl]-N-[(2-methylpropan-2-yl)oxycarbonyl]carbamateHCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 99422504-(Aminomethyl)benzonitrile hydrochloride

実験手順

4-cyanobenzylamine hydrochloride (EX-59A) was prepared from 10 g (0.030 moles) of 4-{N,N-bis-(tert-butoxycarbonyl)aminomethyl}benzonitrile, prepared following Synthetic Communication, 28(23), 4419-4429 (1998), by stirring it in 4N HCl Dioxane (75 ml). After 3 h, the solution was concentraed in vacuo and triturated with ether. The solid was collected by filtration and vacuum dried to yield 5 g (98%) of EX-59A as a white solid: 1H NMR (DMSO) d 8.68 (br s, 2H) 7.84 (m, 2H), 7.67 (m, 2H), 4.06 (s, 2H); HRMS (EI) calcd for C8H8N2 133.0766, found 133.0807.

後処理

  1. customprepared
  2. customtriturated with ether
  3. filtrationThe solid was collected by filtration and vacuum
  4. customdried
  5. customto yield 5 g (98%) of EX-59A as a white solid

出典と根拠

ORDレコード
ord-a94ce1e362de4d3bad6b881d570b3162
出典データセット
uspto-grants-2003_12
特許番号
US06664255B1

関連ノート

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