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

HRID 1733791노트

반응식

HRID 1733791 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a32893798b614d1ca0bd40a25a4b6cb6
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05531978

반응 노트

불러오는 중…