Pyridine → HCID 69012857, 화합물

HRID 1432832노트

반응식

HRID 1432832 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:11]=1[CH2:10][C@H:9]([OH:12])[CH2:8][CH2:7]2.N1C=CC=CC=1.Cl[C:20]([O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:21].C(OC(=O)C)C>C1COCC1>[C:23]1([O:22][C:20](=[O:21])[NH:1][C:2]2[C:11]3[CH2:10][C@H:9]([OH:12])[CH2:8][CH2:7][C:6]=3[CH:5]=[CH:4][CH:3]=2)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 15891Phenyl chloroformateHCID 57936087(2R)-8-Amino-1,2,3,4-tetrahydro-2-naphthalenol

생성물 1

HCID 69012857HCID 69012857, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Next, a solution of (R)-8-amino-1,2,3,4-tetrahydro-naphthalen-2-ol -(36.2 g) and pyridine (18.8 ml) in THF (850 ml) cooled at 0° C. was added phenyl chloroformate (28.8 ml). The mixture was stirred for 3 hours at room temperature, and then poured into ethylacetate. The mixture was washed with aqueous NH4Cl then with water, and the organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. To the obtained residue was added acetonitrile, and the precipitates were collected and washed with a mixture of acetonitrile and diisopropyl ether (2:3) to obtain {(R)-7-Hydroxy-5,6,7,8-tetrahydro-naphthalen-1-yl}carbamic acid phenyl ester (33.0 g).

후처리

  1. washThe mixture was washed with aqueous NH4Cl
  2. dry with materialwith water, and the organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. additionTo the obtained residue was added acetonitrile
  6. customthe precipitates were collected
  7. washwashed with a mixture of acetonitrile and diisopropyl ether (2:3)

출처 및 근거

ORD 기록
ord-1bc980a22fb04358a71adfa1d1c64175
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612113B2

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