Methanol → HCID 67076690、化合物

HRID 2094758ノート

反応式

HRID 2094758 の反応式
[CH3:1][O:2][C:3]([C:5]1([NH:14][C:15](=[O:26])[C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([CH:24]=[O:25])[CH:17]=2)[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6]1)=[O:4].[BH4-].[Na+].CO>C1COCC1>[CH3:1][O:2][C:3]([C:5]1([NH:14][C:15](=[O:26])[C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[C:18]([CH2:24][OH:25])[CH:17]=2)[CH2:6][C:7]2[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH2:13]1)=[O:4]

参加物

5

反応物 3

HCID 887MethanolHCID 4311764Sodium borohydrideHCID 86654801HCID 86654801、化合物

生成物 1

HCID 67076690HCID 67076690、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The compound of step 1 (0.500 g, 1.42 mmol) was dissolved in THF (5 ml) and cooled in an ice bath. Sodium borohydride (0.164 g, 4.25 mmol) was added. Subsequently methanol (2 ml) was added dropwise. After 1 h, the volatiles were evaporated, the residue was partitioned between diethyl ether and a saturated sodium hydrogencarbonate solution, and the aqueous phase extracted with diethyl ether. The combined organic phases were dried over sodium sulfate and evaporated to dryness.

後処理

  1. temperaturecooled in an ice bath
  2. customthe volatiles were evaporated
  3. customthe residue was partitioned between diethyl ether
  4. extractiona saturated sodium hydrogencarbonate solution, and the aqueous phase extracted with diethyl ether
  5. dry with materialThe combined organic phases were dried over sodium sulfate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-075d29933d18414ba4c99aa60e9e1c22
出典データセット
uspto-grants-2013_05
特許番号
US08445530B2

反応ノート

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