[3-(Benzyloxycarbonylamino-methyl)-cyclohexyl]-carbamic acid tert-butyl ester → (3-Amino-cyclohexylmethyl)-carbamic acid benzyl ester

HRID 352212ノート

反応式

HRID 352212 の反応式
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][NH:15][C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[CH2:9]1)(C)(C)C>C(O)(C(F)(F)F)=O>[CH2:19]([O:18][C:16](=[O:17])[NH:15][CH2:14][CH:10]1[CH2:11][CH2:12][CH2:13][CH:8]([NH2:7])[CH2:9]1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

参加物

3

反応物 1

HCID 22713895[3-(Benzyloxycarbonylamino-methyl)-cyclohexyl]-carbamic acid tert-butyl ester

生成物 1

HCID 22714145(3-Amino-cyclohexylmethyl)-carbamic acid benzyl ester

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of [3-(benzyloxycarbonylamino-methyl)-cyclohexyl]-carbamic acid tert-butyl ester (6 g, 16.6 mmol) in TFA (30 mL) was stirred for 1.5 h. The solution was concentrated using benzene to azeotrope, diluted with EtOAc, washed (1.0 N NaOH), dried (Na2SO4), filtered, and concentrated to afford (4.2 g, 97%) as a crude solid. Mass Spectrum (ES+) (m/z) 263.1 [M+1].

後処理

  1. concentrationThe solution was concentrated
  2. additiondiluted with EtOAc
  3. washwashed (1.0 N NaOH)
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford (4.2 g, 97%) as a crude solid

出典と根拠

ORDレコード
ord-11453e1e53c1482a863b7693b5d7aae2
出典データセット
uspto-grants-2004_06
特許番号
US06743794B2

反応ノート

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