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

HRID 37056노트

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HRID 37056 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

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온도
0 °C

실험 절차

5,9-Bis-(benzyloxymethyl)-l-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-6fb69eec706849dc90755d29f9b84f0b
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05419893

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