Acetic Acid → HCID 59805850、化合物

HRID 1429659ノート

反応式

HRID 1429659 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH:5]=O.[CH2:11]1[CH2:20][O:19][C:13]2([CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[O:12]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(O)(=O)C>ClC(Cl)C>[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[F:10])[CH2:5][N:16]1[CH2:17][CH2:18][C:13]2([O:19][CH2:20][CH2:11][O:12]2)[CH2:14][CH2:15]1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 5880883,4-DifluorobenzaldehydeHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 59805850HCID 59805850、化合物収率 98%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

A solution of 3,4-difluorobenzaldehyde (4.40 g, 30.9 mmol), 4,4-ethylenedioxy-piperidine (4.40 g, 30.9 mmol), sodium triacetoxyborohydride (6.40 g, 30.2 mmol) and acetic acid (1.8 g, 30.0 mmol) in dichloroethane (200 ml) was stirred at room temperature for 18 h. After this period, the reaction mixture was washed with 1N sodium hydroxide. The organic layer separated, dried (MgSO4) and the solvents evaporated in vacuo to give D3 (7.9 g, 98%). C14H17F2NO2 requires 269; Found 270 (MH+)

後処理

  1. waitAfter this period
  2. washthe reaction mixture was washed with 1N sodium hydroxide
  3. customThe organic layer separated
  4. dry with materialdried (MgSO4)
  5. customthe solvents evaporated in vacuo

出典と根拠

ORDレコード
ord-973d092066be432e8254e4b43c05a749
出典データセット
uspto-grants-2015_01
特許番号
US08940743B2

反応ノート

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