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Triethylamine → HCID 3625286、化合物

HRID 1031758
ノート
印刷プレビュー

反応式

HRID 1031758 の反応式
C(OC(NC[C@H:10]1[CH2:15][CH2:14][C@H:13]([C:16]([OH:18])=[O:17])[CH2:12][CH2:11]1)=O)(C)(C)C.C([N:21](CC)CC)C.[C:26](Cl)(=O)[O:27][CH2:28][CH3:29].CNC(=O)[C@H](CC1C=CC=CC=1)NC([C@H:39]1[CH2:44][CH2:43][C@H](CNC(OC(C)(C)C)=O)[CH2:41][CH2:40]1)=O>O1CCCC1.CN(C)C=O>[O:27]([C:28]1[CH:29]=[C:15]([CH:10]=[CH:11][CH:12]=1)[CH2:14][CH:13]([C:16]([OH:18])=[O:17])[NH2:21])[C:26]1[CH:43]=[CH:44][CH:39]=[CH:40][CH:41]=1
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 8471Triethylamine2 回HCID 10928Ethyl chloroformateHCID 178453624HCID 178453624、化合物HCID 178485750HCID 178485750、化合物

生成物 1

HCID 3625286HCID 3625286、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

On the other hand, trans-4-(t-butoxycarbonylaminomethyl)cyclohexylcarboxylic acid (1.62 g) was dissolved in dry tetrahydrofuran (50 ml) and N,N-dimethylformamide (20 ml), triethylamine (0.96 ml) was added, and a solution of ethyl chlorocarbonate (0.76 g) in dry tetrahydrofuran (2 ml) was added, followed by stirring for 30 minutes. To the solution, the previous hydrochloride (III) and triethylamine (2 ml) was added, and the mixture was stirred under room temperature for 3 hours. Ice-water (200 ml) was added to the reaction mixture, and the precipitated crystalline substance was collected by filtration, thoroughly washed with water, and dried to obtain 2.62 g of N-[trans-4-(t-butoxycarbonylaminomethyl)cyclohexylcarbonyl]-3-phenoxy-DL-phenylalanine 4-acetylanilide (IV). The NMR data did not contradict this result.

後処理

  1. stirringthe mixture was stirred under room temperature for 3 hours
  2. filtrationthe precipitated crystalline substance was collected by filtration
  3. washthoroughly washed with water
  4. customdried

出典と根拠

ORDレコード
ord-30756c4412b04ee5bfcd755dc2977396
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954512

反応ノート

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