Pyridine → HCID 69012857、化合物

HRID 1432832ノート

反応式

HRID 1432832 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 69012857HCID 69012857、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-1bc980a22fb04358a71adfa1d1c64175
出典データセット
uspto-grants-2009_11
特許番号
US07612113B2

反応ノート

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