Sodium borohydride → Tricyclohexylstannane

HRID 501919

反応式

HRID 501919 の反応式
C(OCC)C.O.[BH4-].[Na+].[OH-].[CH:10]1([Sn+:16]([CH:23]2[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]2)[CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1>C(OCC)C>[CH:23]1([SnH:16]([CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15]2)[CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][CH2:18]2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]1

参加物

5

反応物 3

HCID 4311764Sodium borohydrideHCID 9864905CyhexatinHCID 21584184Diethylether water

生成物 1

HCID 25729Tricyclohexylstannane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture (400 mL) of diethyl oxide:water 1:1 was cooled at 0° C. under nitrogen in a three-necked flask of 1 L. Sodium borohydride (3 g, 79.4 mmol) and then tricyclohexyltin hydroxide (30 g, 62.2 mmol) were successively and carefully added. After addition of 100 mL of diethyl oxide, the mixture was stirred 2 days at room temperature. After separation, the organic layer was dried over magnesium sulphate and evaporated under reduced pressure. The crude product was distilled under high vacuum to afford, a colourless oil (23.23 g; 63 mmol).

後処理

  1. additioncarefully added
  2. customAfter separation
  3. dry with materialthe organic layer was dried over magnesium sulphate
  4. customevaporated under reduced pressure
  5. distillationThe crude product was distilled under high vacuum
  6. customto afford

出典と根拠

ORDレコード
ord-e9984706c97648daa4d4da5956ff6f64
出典データセット
uspto-grants-2010_08
特許番号
US07772417B2

関連ノート

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