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Trifluoroacetic acid → HCID 71554976、化合物

HRID 2281672
ノート
印刷プレビュー

反応式

HRID 2281672 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[C:14]3([CH2:17][N:16]([C:18](OC(C)(C)C)=[O:19])[CH2:15]3)[CH2:13][CH2:12]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.FC(F)(F)C(O)=O.[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][N:41]=C=O.C(N(CC)CC)C>ClCCl.C(#N)C>[Cl:32][C:33]1[CH:38]=[C:37]([Cl:39])[CH:36]=[CH:35][C:34]=1[CH2:40][NH:41][C:18]([N:16]1[CH2:15][C:14]2([N:11]([S:8]([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)(=[O:9])=[O:10])[CH2:12][CH2:13]2)[CH2:17]1)=[O:19]
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 6422Trifluoroacetic acid2 回HCID 8471TriethylamineHCID 46127082,4-Dichlorobenzyl isocyanateHCID 86682348HCID 86682348、化合物

生成物 1

HCID 71554976HCID 71554976、化合物収率 91.1%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile
溶媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptane-6-carboxylate (452 mg, 1.27 mmol) in dichloromethane (8 mL) was added trifluoroacetic acid (489 μl, 6.34 mmol). After 2 h at ambient temperature, another amount of trifluoroacetic acid was added (300 μl, 3.89 mmol). The reaction mixture was stirred for 1.5 h at ambient temperature and concentrated under reduced pressure. The residue was partitioned in toluene (10 mL) and then concentrated, this procedure was repeated twice to give the unpurified amine (540 mg), which was used directly in the next step without further purification. To a solution of the obtained 1-(4-fluorophenylsulfonyl)-1,6-diazaspiro[3.3]heptanes in acetonitrile (10 mL) was added 2,4-dichloro-1-(isocyanatomethyl)benzene (216 μl, 1.47 mmol) followed by triethylamine (294 μl, 2.11 mmol) and the mixture was stirred for 1 h at ambient temperature. The solvent was evaporated in vacuo and the resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5) to give the titled compound (530 mg, 91%) as colorless solid. HRMS (EI): 457.0431 (exact mass calculated for C19H17Cl2FN3O3S ([M]+)=457.0430).

後処理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was partitioned in toluene (10 mL)
  3. concentrationconcentrated
  4. customto give the unpurified amine (540 mg), which
  5. customwas used directly in the next step without further purification
  6. stirringthe mixture was stirred for 1 h at ambient temperature
  7. customThe solvent was evaporated in vacuo
  8. customthe resulting solid was purified by chromatography (SiO2; heptane:ethyl acetate 1:4 to dichloromethane/methanol/ammonia 95:4.5:0.5)

出典と根拠

ORDレコード
ord-d2261def993a4c32bb6bf5fda3f9e2fa
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09139593B2

反応ノート

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