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Iodine → 2-Amino-2-(4-chlorophenyl)ethan-1-ol

HRID 423043
ノート
印刷プレビュー

反応式

HRID 423043 の反応式
[CH3:1][S:2]([O:5][CH2:6][CH:7]([NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)(=[O:4])=[O:3].[NH2:23][CH:24]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=1)[C:25](O)=[O:26].[BH4-].[Na+].II>C1COCC1>[CH3:1][S:2]([O:5][CH2:6][CH:7]([NH:15][C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[C:8]1[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=1)(=[O:3])=[O:4].[NH2:23][CH:24]([C:28]1[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][CH:29]=1)[CH2:25][OH:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 807IodineHCID 587821Benzeneacetic acid, alpha-amino-4-chloro-HCID 4311764Sodium borohydrideHCID 577502782-(Tert-butoxycarbonylamino)-2-(4-chlorophenyl)ethyl methanesulfonate

生成物 2

HCID 148531952-Amino-2-(4-chlorophenyl)ethan-1-ol収率 11.88%
HCID 57750278
2-(Tert-butoxycarbonylamino)-2-(4-chlorophenyl)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

The tert-butyl 1-(4-chlorophenyl)-2-hydroxyethylcarbamate used in the above reaction was prepared as follows. 2-Amino-2-(4-chlorophenyl)acetic acid (12 g, 64.65 mmol) was stirred in THF (200 mL) and sodium borohydride (5.82 g, 153.87 mmol) was added in portions to the stirred mixture under nitrogen. A solution of iodine (16.41 g, 64.65 mmol) in THF (20 mL) was added dropwise maintaining the temperature below 15° C. using an ice bath. The resulting mixture was warmed to room temperature and stirred at reflux overnight. The reaction was quenched by the addition of methanol (40 mL). A portion of this solution was removed (50 mL) and partitioned between ethyl acetate and water. The organic layer was concentrated under reduced pressure. The residue was purified by MPLC on silica using gradient elution (0 to 10% methanol/DCM). The desired product, 2-amino-2-(4-chlorophenyl)ethanol (1.318 g, 11.88%), was thus isolated as a colourless solid.

後処理

  1. customwas prepared
  2. temperaturemaintaining the temperature below 15° C.
  3. temperatureat reflux overnight
  4. customThe reaction was quenched by the addition of methanol (40 mL)
  5. customA portion of this solution was removed (50 mL)
  6. custompartitioned between ethyl acetate and water
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. customThe residue was purified by MPLC on silica using gradient elution (0 to 10% methanol/DCM)

出典と根拠

ORDレコード
ord-5a5d84c282d3452bb8ddb737e69c9c3e
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08101623B2

反応ノート

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