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Water → HCID 178453662、化合物

HRID 1159391
ノート
印刷プレビュー

反応式

HRID 1159391 の反応式
[OH:1][C@@H:2]1[CH2:5][C@H:4]([CH2:6][NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11])[CH2:3]1.C(N(CC)CC)C.[CH3:22][S:23](Cl)(=[O:25])=[O:24].O>C(Cl)Cl>[CH3:22][S:23]([O:1][C@H:2]1[CH2:5][C@@H:4]([CH2:6][NH:7][C:8]([O:9][C:10]([CH3:11])([CH3:13])[CH3:12])=[O:14])[CH2:3]1)(=[O:25])=[O:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 178453655HCID 178453655、化合物

生成物 1

HCID 178453662HCID 178453662、化合物収率 70%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Intermediate 29, tert-Butyl [(cis-3-Hydroxycyclobutyl)methyl]carbamate (5.15 g, 26 mmol) and triethylamine (8.9 mL, 61 mmol) were dissolved in CH2Cl2 (50 mL). MsCl (2.4 mL, 31 mmol) was added dropwise at −20° C. under stirring in argon. The temperature was brought to ambient within 1 h. Water (100 mL) was added, and the layers were separated. The organic one was washed with water, brine, dried with Na2SO4, and evaporated, to give the title compound (5 g, 70%) white crystals. This crude product was used for the next stage without additional purification. 1H NMR-data (DMSO-d6): 6.74-7.00 (m, 1H, NH); 4.73-4.86 (m, 1H); 3.10 (s, 3H, MS); 2.97 (t, 2H, CH2, J=5.7 Hz); 2.32-2.42 (m, 2H); 1.80-2.43 (m, 3H); 1.38 (s, 9H, Boc).

後処理

  1. customthe layers were separated
  2. washThe organic one was washed with water, brine
  3. dry with materialdried with Na2SO4
  4. customevaporated

出典と根拠

ORDレコード
ord-807cd78fdc2d4474b3d61f6ed8dea735
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07812040B2

反応ノート

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