Hydrochloric Acid → 5,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane

HRID 1733791ノート

反応式

HRID 1733791 の反応式
[CH2:1]([O:8][CH2:9][CH:10]1[CH2:21][NH:20][CH2:19][CH:18]([CH2:22][O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[NH:17][C:16](=O)[CH2:15][O:14][CH2:13][C:12](=O)[NH:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>O1CCCC1>[CH2:24]([O:23][CH2:22][CH:18]1[CH2:19][NH:20][CH2:21][CH:10]([CH2:9][O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[NH:11][CH2:12][CH2:13][O:14][CH2:15][CH2:16][NH:17]1)[C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 194385105,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione

生成物 1

HCID 194385445,9-Bis(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

5,9-Bis-(benzyloxymethyl)-1-oxa-4,7,10-triazacyclododecane-3,11-dione (0.250 g, 0.566 mmol) was dissolved in dry tetrahydrofuran (10 ml) cooled to 0° C. A 1M solution of borohydride-THF complex in tetrahydrofuran (5 ml) was added under nitrogen and the mixture was stirred at ambient temperature for 14 hours. 2M Hydrochloric acid (3 ml) was added and the mixture was concentrated in vacuo to approximately 1 ml volume. 25% Ammonia solution (2 ml) was added and the mixture was extracted four times with 4 ml of chloroform. The extracts were concentrated in vacuo and gave a yellow oil which showed an absence of carbonyl bands in IR. Yield 0.227 g (97%), FAB MS: 414 (M+1).

後処理

  1. concentrationthe mixture was concentrated in vacuo to approximately 1 ml volume
  2. addition25% Ammonia solution (2 ml) was added
  3. extractionthe mixture was extracted four times with 4 ml of chloroform
  4. concentrationThe extracts were concentrated in vacuo
  5. customgave a yellow oil which

出典と根拠

ORDレコード
ord-a32893798b614d1ca0bd40a25a4b6cb6
出典データセット
uspto-grants-1996_07
特許番号
US05531978

反応ノート

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