1,2-Dichloroethane → HCID 69821478, 화합물

HRID 2186659

반응식

HRID 2186659 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][CH2:11][C:12]([OH:14])=O)=[CH:5][CH:4]=1.C(N(CC)CC)C.C(Cl)CCl.[NH2:26][C@@H:27]([CH2:36][N:37]1[CH2:42][CH2:41][O:40][CH2:39][CH2:38]1)[C@H:28]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[OH:29]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][CH2:11][C:12]([NH:26][C@@H:27]([CH2:36][N:37]2[CH2:38][CH2:39][O:40][CH2:41][CH2:42]2)[C@H:28]([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)[OH:29])=[O:14])=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 782804-(4-Methoxyphenyl)butyric acidHCID 10513992(1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol

생성물 1

HCID 69821478HCID 69821478, 화합물수율 66.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Methylene chloride (10 ml), 4-(4-methoxyphenyl)butanoic acid (388.0 mg, 2.0 mmol), triethylamine (0.70 ml, 5.0 mmol) and EDC (580 mg, 3.0 mmol) were added to (1S,2S)-2-amino-3-morpholino-1-phenyl-1-propanol (472.0 mg, 2.0 mmol), followed by stirring overnight. Methylene chloride (100 ml) was added to the reaction solution. After washed with a saturated sodium hydrogen carbonate solution (50 ml), water (50 ml) and saturated brine (50 ml) successively, the organic layer was dried over sodium sulfate and filtered, and the solvent was evaporated under reduced pressure. The resulting crude product was purified by silica gel column chromatography (chloroform:ethanol=20:1) to obtain the title compound (549 mg, yield 66%) as colorless oil.

후처리

  1. washAfter washed with a saturated sodium hydrogen carbonate solution (50 ml), water (50 ml) and saturated brine (50 ml) successively
  2. dry with materialthe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. customthe solvent was evaporated under reduced pressure
  5. customThe resulting crude product was purified by silica gel column chromatography (chloroform:ethanol=20:1)

출처 및 근거

ORD 기록
ord-b04c55622f534f38b9fb8bc490f9daf4
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06407064B2

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