Hydrogen Bromide → HCID 178462028, 화합물

HRID 1252525노트

반응식

HRID 1252525 반응식
C(OC([NH:11][C@@H:12]([CH2:33][C:34](=[O:53])[NH:35]C(C1C=CC(OC)=CC=1)C1C=CC(OC)=CC=1)[C:13]([NH:15][C@H:16]([C@@H:20]([NH:22][C@H:23]([C:30]([OH:32])=[O:31])[CH2:24][C:25]1[N:26]=[CH:27][NH:28][CH:29]=1)[CH3:21])[C:17]([OH:19])=[O:18])=[O:14])=O)C1C=CC=CC=1.Br.C(OCC)(=O)C>C(O)(=O)C>[NH2:11][C@@H:12]([CH2:33][C:34](=[O:53])[NH2:35])[C:13]([NH:15][C@H:16]([C@@H:20]([NH:22][C@H:23]([C:30]([OH:32])=[O:31])[CH2:24][C:25]1[N:26]=[CH:27][NH:28][CH:29]=1)[CH3:21])[C:17]([OH:19])=[O:18])=[O:14]

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 8857Ethyl AcetateHCID 178491198HCID 178491198, 화합물

생성물 1

HCID 178462028HCID 178462028, 화합물수율 59%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of (2R,3S)-2-[[(2S)-2-benzyloxycarbonylamino-3-[N-[bis(4-methoxyphenyl)methyl]carbamoyl]propionyl]amino]-3-[[(1S)-1-carboxy-2-(4-imidazolyl)ethyl]amino]butyric acid (635 mg) and 30% hydrogen bromide in acetic acid (5 ml) was stirred for 2 hours at room temperature and the mixture was poured into a mixture of ice-water (20 ml) and ethyl acetate (20 ml). The aqueous phase was separated and subjected to a column of Dowex 50W x 8 (H+, 20 ml). The column was washed with water and the elution was carried out with 2.8% aqueous ammonia. The object fractions were collected and evaporated in vacuo. The residue was dissolved in water (50 ml) and lyophilized to give (2R,3S)-2-[[(2S)-2-amino-3-carbamoylpropionyl]amino]-3-[[(1S)-1-carboxy-2-(4-imidazolyl)ethyl]amino]butyric acid (190 mg) as a white powder.

후처리

  1. customThe aqueous phase was separated
  2. washThe column was washed with water
  3. washthe elution
  4. customThe object fractions were collected
  5. customevaporated in vacuo
  6. dissolutionThe residue was dissolved in water (50 ml)

출처 및 근거

ORD 기록
ord-7a1d5cf4936846a399f2249577730946
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04743614

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